Research ArticleAntibacterial Finishing of Cotton Fabric Using Stinging Nettle(Urtica dioica L) Plant Leaf Extract
Asnake Ketema and Amare Worku
Ethiopian Institute of Textile and Fashion Technology Bahir Dar University Bahir Dar Ethiopia
Correspondence should be addressed to Amare Worku amareworku2005ddueduet
Received 14 January 2020 Revised 22 February 2020 Accepted 31 March 2020 Published 21 April 2020
Academic Editor Hakan Arslan
Copyright copy 2020 Asnake Ketema and Amare Worku +is is an open access article distributed under the Creative CommonsAttribution License which permits unrestricted use distribution and reproduction in anymedium provided the original work isproperly cited
Natural organic fibers such as cotton linen and wool are readily attacked by microorganisms Microbial growth on a textile fabriccauses loss of strength and elongation discoloration and changes in appearance+e antibacterial finishing agents extracted fromnettle plant leaf have been used to impart finish to the cotton fabric by using the Pad-Dry-Cure application method +eantibacterial activity of the finish was assessed quantitatively using the AATCC 1002004 test method and the antibacterial activityagainst Gram-positive (Staphylococcus aureus) and Gram-negative (Escherichia coli) bacteria was measured +ere was a 100 to9975 percent reduction in the count of test bacteria Physical properties of treated and untreated cotton fabrics such as ab-sorbency fabric stiffness air permeability and strength were analyzed To evaluate the laundering effect of stinging nettle leaffinished fabric samples were subjected to laundry with 5 10 15 20 25 30 35 and 40 washing cycles using standard AATCC testmethod 61 and bacterial count of treated samples was tested+e results showed gradual decrease in antibacterial property with a100 to 44 reduction in the bacterial count for Staphylococcus aureus and a 100 to 30 reduction in the bacterial count forEscherichia coli +e results of this investigation suggested that nettle leaf a low-cost abundant plant in Ethiopia can be used forantibacterial activity in woven cotton fabric
1 Introduction
Certain textile material treatments are applied to improvethe look and qualities of textile goods +ese treatments arecalled finishes A finish is a treatment given to a piece offabric to change appearance handlingtouch or perfor-mance +e purpose is to make the fabric more suitable forits end use +e finishes may be basic or functional Basicfinishes also called aesthetic finishes are applied to almostall the fabrics to improve their appearance feel and bodyFunctional finishes are applied to improve the performanceof fabric for some specific purpose for example fireproofwaterproof bulletproof crease-resistant and antimicrobialfinishes [1]
Bacteria either pathogenic or not are normally found onhuman skin nasal cavities and other areas such as thegenital area [2 3] Typically pathogenic bacteria like
Escherichia coli and Staphylococcus aureus have been foundon textiles [4] +e negative role of microorganisms in thetextiles leads the researchers to the development of textileswith antibacterial properties With this growth in healthawareness many people focused their attention on edu-cating themselves about and protecting themselves fromharmful pathogens [5ndash7] It soon became more vibrant forantibacterial finished textiles to protect the user from bac-teria rather than simply protecting the garment from fiberdegradation [8] Requirements for antimicrobial agents ontextiles concern safety (producer and user) wash and heatfastness and applicability without negative effects on thetextile properties
Besides antimicrobial textiles should maintain textileproperties such as appearance feel and durability tolaundering as new functional treatment is fabricated becausethese are important to the consumer +erefore new
HindawiJournal of ChemistryVolume 2020 Article ID 4049273 10 pageshttpsdoiorg10115520204049273
advanced and innovative technologies are required Severalchemicals have been employed to impart antimicrobialactivity to textile goods +ose chemicals embrace inorganicsalts organ metallics iodophors (substances that slowlyrelease iodine) phenols and thiophenols antibiotics het-erocyclic and anionic groups and related compoundsformaldehyde derivatives and amines Many of thesechemicals however are toxic to humans they do not easilydegrade in the environment [9 10] Although chemicalantimicrobials are effective against a wide range of microbesthey are cause of concern due to the associated side effectsand water pollution +e use of synthetic products is be-coming increasingly problematic leading to microbial re-sistance product withdrawal undesirable environmentalproblems and animal toxicity [11ndash14] Hence there is agreat demand for antimicrobial treated textiles based on eco-friendly agents helping to effectively reduce the ill effectsassociated with microbial growth on textile material[11 15ndash20] +e use of natural plant products for antimi-crobial finishing of textile materials has been widely re-ported+ere are vast sources of medicinal plants with activeantimicrobial ingredients such as tulsi pomegranate andeucalyptus [21] +e research on their use in textiles is verylimited and not well documented+ese natural products areassociated with various benefits like lower incidence ofadverse reactions and reduced cost compared to syntheticpharmaceutical products and can be exploited as an at-tractive eco-friendly alternative to synthetic antimicrobialagents for textile applications [22 23]
Ginkgo-Biloba extract is an eco-friendly antimicrobialagent and its application was investigated in health andmedicinal purposes Due to its nontoxicity characteristics itis a potential candidate for antimicrobial finishing of in-stitutional textiles range including home accessories hos-pital bed sheets nursesrsquo uniforms and surgical gowns anddrapes+e plant-based natural fruit source was reported forits antimicrobial properties the fruit-based source is pine-apple (Ananas comosus) whose juice was investigated for itsactivity against harmful microbes +e antimicrobial activitywas evaluated through the agar diffusion method Anotherplant-based source reported is papaya (Carica papaya) [2425] Berberis vulgaris L wood as an agricultural waste wasused for dyeing and functional finishing of cotton To fa-cilitate the attachment of natural dye citric acid was used tocreate carboxylic acid functional groups on cotton fibers+e dyed sample prepared under the optimum conditions ofcrosslinking showed good wash and light fastness propertiesbesides very good antibacterial activity against Gram-neg-ative and Gram-positive bacteria [26]
+e chitosan and alginate have been used for antimi-crobial finishing of textiles Chitosan is a derivate of chitin itis water-soluble and cellulose-based Chitin is a polysac-charide based on amino sugars In an acid solvent the aminecomponent turns into a quarterly amino unit that inhibitsthe growth of microbes +is amino unit works as a shield toblock the protein and slow down proliferation by distractingcell membrane this permits the substance to escape from thebacterial cell resulting in the death of the bacteria Anti-microbial activity of chitosan was reported in many studies
and it is a widely accepted antimicrobial agent [8] Severalnatural agents such as basil (with active agent being euge-nol) neem (with active limonoids like azadirachtin nim-binin) turmeric (curcumin) clove oil chitosan sericinonion aloe vera and pomegranate have antimicrobialproperties [27 28]
Natural dye is now fast growing compared to syntheticdye for its safe healthy and eco-friendly nature and ap-plication Extraction and utilization of natural pigmentshave received broad attention in the current years Kapokflower is an unexplored source of natural dyestuff which canalso be utilized for the functionalization of cellulose-basedtextiles [29] Kapok flower extract (KFC) was utilized as afunctional dye for dyeing of linen fabric in the presence ofmetallic mordants +e dyed fabrics were assessed for col-oration properties (color values color coordinates andfastness properties) as well as functional properties such asantibacterial activity UV protection and antioxidant ac-tivity +e dyed fabrics displayed an excellent antibacterialactivity against Gram-positive and Gram-negative bacteria[2]
+e coloration of wool by kapok flower extract (KFE) bytannin-based natural mordant using premordanting treatingtechnique could impart important functional properties tothe dyed fabrics Wool fabrics were mordanted usingtamarind seed coats extract (TSCE) and further dyed withKFE +e dyed fabrics were evaluated for coloration prop-erties (color values fastness properties) as well as functionalproperties like antibacterial and antioxidant activity [30]Flora forest is a major component that contributes to thenatural resources from which natural pigment can be de-rived Both silk and wool showed excellent dyeing abilitywhen dyed with the extracted pigments Fabrics dyed withleaf pigments showed an unchanged or increased color-fastness to light washing and storage +is is because therich content of phenolic hydroxyl within leaf chemicalstructure is sensitive to light and alkaline condition and canresult in a hyperchromic effect [31] +e natural dyes requiremordants for their fixation on textile materials Naturalmordants are thus gaining importance in order to getcomplete-natural dyeing +e natural mordants namelyhard and tamarind seed coat and natural dyes like turmericand henna were extracted using conventional and ultra-sound approaches and various extracts obtained were de-scribed in terms of their optical densities +e combinationsof mordantsdyes and dyed fabrics were evaluated for theircolor strength and fastness properties [32]
Stinging nettle (Urtica dioica L) is grown in many areasacross the world annually It belongs to medicinal herbs [33]Several findings show that the stinging nettle (Urtica dioicaL) plant contains compounds like alkaloids phenols sa-ponins steroids tannins and glycosides which exhibit an-timicrobial properties [15] +e leaf extracts of nettle (Urticadioica) were studied and reported to have excellent anti-microbial activity against microorganisms based on theavailability of large amounts of bioactive compounds such astannins flavonoids and alkaloids which are effective againstbacterial and fungal infections [9] With respect to that theuse of nettle (Urtica dioica) leaf extract as a textile finish on
2 Journal of Chemistry
cotton fabrics has not been examined and reported in anyform
In the current study the interaction of extracted com-ponents from the nettle plant leaf with cotton fabric usingcitric acid and their potential antimicrobial efficacy againstStaphylococcus aureus and Escherichia coli bacterial specieswhich are known to cause cross infections in the cottonfabric as well as being responsible for causing unpleasantodors in textiles were investigated
2 Materials and Methods
21 Materials and Apparatus Citric acid was used as aprecursor for the crosslinking agent between extractedpowder and fabric Ethanol (CH3CH2OH 97 purity) wasprepared according to the procedure needed for the ex-traction of chemical ingredients from the nettle leaf
A hundred percent of scoured cotton fabric was used inthis study to ensure complete wetting and uniform absor-bency of the solution during padding Scouring treatmentwas applied to the woven cotton fabric to remove foreignmaterial before imparting antibacterial finish
+e following apparatus was used in this study ultra-sonic extractor electronic balance oven dryer Whatmanfilter paper No 1 pHmeter measuring cylinder Condensermagnetic stirrer crucible muffle furnace FTIR TGA UVspectroscopy and padding mangle
22 Preparation of Sample +e plant leaf was collected fromAmhara region in Debre Tabor Ethiopia and washed withpure water rinsed with distilled water cleaned air-dried for8 days and cut into small pieces for further size reductioninto fine powder with the help of electric grinder up to0710 μm particle size Major phenolic chemical ingredientsof nettle leaf extract are given in Figure 1
23 Ultrasonic Extraction Technique Ultrasonic assistedextraction (UAE) method has been considered according toits simplicity to extract the responsible chemical com-pounds easy handling low cost high yield or efficiencylower organic extraction solvent consumption reduced timefor extraction and reliable procedure in an extensive rangeof organic solvents for various phenolic compounds in large-scale level and industry Air-dried nettle leaf sample 20grams was prepared in 200ml 400ml and 600ml of waterand 975 ethanol and extracted using ultrasonic extractiontechniques for 30 60 and 90 extraction minutes at 45ndash50degC(Table 1) +e extracted ingredient was filtered through afilter paper (Whatman No 1) which was impregnated withthe same solvents +e ethanol was concentrated to neardryness under reduced pressure below 50degC using a rotaryevaporator machine +e amount of the concentrated in-gredient extracted was noted down and stored in air tightglass bottles in a refrigerator until further use [35]
Based on the parameters in Table 2 antibacterial agentwas extracted and the number of trials is designed andgenerated using central composite design (CCD) Design-Expertreg version 11 software
24 Quantitative Phytochemical Analysis +e leaf extractthat exhibited the maximum antibacterial activity wasassessed for the presence of phytochemicals A preliminaryphytochemical analysis was performed to determine theamount of phenolic and flavonoid compounds in milligramper gram of extracted powder [36ndash38]
25 Determination of Total Phenolic Content (TPC)UV-spectrophotometric methods are most commonly usedfor the quantification of phenolic content Preparation ofstandard gallic acid solution was as follows 02 gram of gallicacid was dissolved into 200ml distilled water so the con-centration of the solution was 0001 gramml or 1000 microgml+is is called the stock solution +en serial dilution wasperformed in order to prepare different concentrations ofthe solution (0 gml 50 gml 100mgml 150mgml200mgml 250mgml and 300mgml) which are used forpreparing calibration curve
Estimation of total phenol content in the selected plantextract was measured spectrophotometrically byFolinndashCiocalteu (FCR) colorimetric method using gallicacid as the standard and expressing results as gallic acidequivalent (GAE) per gram of sample Different concen-trations (001mgml) of gallic acid were prepared inmethanol Aliquots of 1ml of the test sample and eachsample of the standard solution were taken and mixed with2ml of FolinndashCiocalteu reagent (1 10 in deionized water)and 4ml of a saturated solution of sodium carbonate (75wv) +e tubes were covered with silver foils and incubatedat room temperature for 30 minutes with intermittentshaking +e absorbance was taken at 765 nm using meth-anol as blank All the samples were analyzed in three rep-lications +e total phenolic amount was determined withthe help of a standard cure prepared from a pure phenolicstandard (gallic acid) [10 39 40]
TPCmgGAE
m1113874 1113875
ClowastV
m (1)
A formula was used to assess the phenolic compoundsin mg from one gram of extracted powder when the TPCamount increases the antibacterial activity will be effective
Here TPC is the total phenol content in mg of gallic acidequivalent per gram of extracted gallic acid equivalent m isdry mass of a sample in gram used for characterization C is aconcentration of gallic acid in mgl and V is the volume ofsample taken in a milliliter
26 Determination of Total Flavonoid Content (TFC) +eTFC of the leaf extract was determined by aluminumchloride colorimetric assay Briefly 05ml aliquots of theextract and standard solution (001ndash10mgml) of quercetinwere added to 2ml of distilled water and subsequently to015ml of sodium nitrite (5 NaNO2 wv) solution andmixed After 6 minutes 015ml of (10 AlCl3 wv) solutionwas added+e solutions were allowed to stand for quercetin6min and after that 2ml of sodium hydroxide (4 NaOHwv) solution was added to the mixture +e final volumewas adjusted to 5ml with immediate addition of distilled
Journal of Chemistry 3
water mixed thoroughly and allowed to stand for another15min +e absorbance of each mixture was determined at510 nm against the samemixture but without leaf extract as ablank TFC was determined as mg quercetin equivalent pergram of sample with the help of the calibration curve ofquercetin All measurements were performed in triplicate(n 3) [41]
TFCmgQUE
m1113874 1113875
ClowastV
m (2)
+e total flavonoid content of the extracts can be de-termined using the above formula where C is the concen-tration of quercetin in mgL of quercetin equivalence V isthe volume of sample taken (ml) m is the dry weight of
sample (g) and TFC is the total flavonoid content in mg ofquercetin equivalence
27 Functional Group and 4ermal Analysis FourierTransform Infrared (FTIR) Spectrophotometer is the mostpowerful tool for identifying the types of functional groupsbased on the wavelength of light absorbed By interpretingthe infrared absorption spectrum the chemical bonds in amolecule were determined [42]
+e TGA curve was obtained with a heating rate of10degCminminus1 in the temperature range of 30 to 1000degC byusing alumina crucibles and samplesrsquo mass of about 10mg+e experiments were carried out under the nitrogen at-mosphere at a flow rate of 50mlminminus1
28 Application Procedure Pad-Dry-Cure is most widelyused for 100 scoured cotton fabric Nettle leaf extractedpowder was treated with nine percent on weight of fabric(owf) under room temperature +e treated fabric waspassed between the rollers two to three times at a uniformpressure at 15 bar for better penetration of finishing agentand to squeeze out excess liquid from the fabric +e fabricwas then dried at 110degC and cured at 130degC in a curingchamber within 3 minutes
29 Antibacterial Test Antibacterial testing was done byAATCC standard test method 1002004 for the quantitativevaluation of the antibacterial effectiveness of the antimi-crobial agents against Gram-positive bacteria (Staphylo-coccus aureus) and Gram-negative bacteria (Escherichiacoli) Assessment of the percent reduction of bacteria wascalculated using
R() B minus A
B1113874 1113875 times 100 (3)
R is the percent reduction of bacteria A is the thenumber of bacteria recovered from the inoculated treatedtest specimen swatches in the jar incubated over the desiredcontact period B is the the number of bacteria recoveredfrom the inoculated untreated test specimen swatches in thejar incubated over the desired contact period microbes anddyed fabric
HO
HO
OH
OH
O
O
O
O
(a)
HO
HOHO
HO
OH
OH
OH
OH
H3C
OH
OH
O
OO
O
O
O
(b)
Figure 1 Chemical structures of extracted phenolic compound (a) 2-O-caffeoylmalic acid (b) rutin [33 34]
Table 1 Antibacterial agent extraction parameters water andethanol used as extraction solvents
Extraction factors ParametersMaterial to liquor ratio 1 10 1 20 1 30Extraction time (minutes) 30 60 90Extraction temperature (degC) 45ndash50
Table 2 Number of runs by using central composite design (CCD)and their yield
210 Wash Durability Test +e treated fabrics were laun-dered using AATCC test method 61 Laundering was carriedout at MLR of 1 10 with 05 on weight of fabric of AATCCdetergent and 100 steel balls at a temperature of 90degC for 30minutes +e washing cycle was followed by hot rinsing inplain water at 40degC for 10 minutes Finally the washedswatches were tumble-dried Since a single wash-dry cyclesimulated 8 regular wash cycles the laundering procedurewas repeated 5 10 15 20 25 30 35 and 40 times to checkchemical durability
3 Results and Discussion
31 Yield of Extraction Using Water and Ethanol +e ex-perimental results (Table 2) can be illustrated by the fol-lowing linear equation
Yield 1015076 + 033 time + 0497487 conc (4)
Yield 1498065 + 031 Time + 0497487Conc (5)
Equations (4) and (5) depict the yield that has a linearrelationship with the factor of extraction time and con-centration of water and ethanol used as extraction solventrespectively
+e actual value and model prediction value of the yieldshowed a good correlation (Figure 2) Based on the ANOVAanalysis the linear equation has a p-value of 00001 (lt005)indicating that the equation model is significant
32 Analysis of Variance (ANOVA) +e results of theANOVA analysis factors A and B had a significant effect(Tables 3 and 4) +e factors A and B had a p-value of 00001and 00001 respectively +e model showed that the factorsA and B had a positive effect on the extraction yield indi-cating an increase in these factors extraction yield increases(Figure 3)
33 Optimization Extraction Parameters +e optimumconditions are based on the resulting desirability value +egoal of extraction is to minimize extraction time concen-tration and maximum water and ethanol extraction yield asshown in Tables 5 and 6 respectively +e optimizationprocess was performed by establishing the highest level ofextraction yield
Table 7 shows that the optimal extraction time is 59minutes with concentration of 10mlg the predictiveyield is 34991 percent Ethanolic extraction yield hasoptimal extraction time of 59026 minute with concen-tration of 10458mlg the predictive yield is 38716percent (Table 8)
34 Quantitative Analysis of Phytochemical Ingredients+e amount of total phenol content in the extract was de-termined by the Folin-Ciocalteau reagent described in theMaterials and Methods section using gallic acid as thestandard +e absorbance values obtained at differentconcentrations of gallic acid were used for the construction
of a calibration curve It appeared that the extraction ofnettle plant leaf total phenolic content is 27819plusmn 0131mgGAEg dry weight (equation (1))+e total flavonoid contentin the extract of nettle plant leaves is 2566plusmn 0227mgGAEgdry weight (equation (2)) [43ndash46]
FTIR studied in extracted nettle leaf displayed strongabsorption peaks at 307819 cmminus1 154929 cmminus1 140509 cmminus1and 107781 cmminus1 +e broad peak between 3500 cmminus1 and2500 cmminus1 corresponds to a strong O-H stretch vibrationwhich indicates the presence of hydroxyl groups in nettle leafextract On finger print region a doublet band is presentbetween1390 cmminus1 and 1310 cmminus1 representing O-H bendingwhich indicates phenolic compounds +e FTIR spectra of thetreated and untreated cotton fabric were almost the same andslight differences were at wave number 3000ndash2500 cmminus1 +etreated fabric has O-H stretch vibration and OH functionalgroup between 3000 and 2500 cmminus1 (Figure 4(a))
+e TGA curves of the crude extract showed that asmall weight loss was found in the range of 90ndash162degC dueto the evaporation of the humidity of the materials orvolatile compounds 162ndash537degC was associated with ali-phatic phenolic compounds decomposition or degrada-tion Char formation was detected between 537 and1028degC by further extending the analysis temperature(Figure 4(b))
35 Effect of Tensile Strength +e tensile strength of the Pad-Dry-Cure treated cotton fabric decreased by 066 and 117percent compared to the untreated control in warp and weftdirection respectively
Other physical properties such as permeability stiffnessstrength and absorbency were tested accordingly based onASTM ISO and AATCC standard respectively [33 47]
36 ReactionMechanisms +e two carboxylic groups of thecitric acid are linked with the hydroxyl part of the celluloseand with extracted phenol through covalent bond (Figure 5)+eir effective antibacterial activity and phenolic com-pounds were attached to cotton fabric using citric acid as acrosslinker Phenolic compounds are among the major anddiverse groups of active compounds in the nettle plant leafCotton fabrics treated with phenolic compounds showedexcellent antibacterial activity against the Gram-positivebacteria Staphylococcus aureus as well as the Gram-negativebacteria Escherichia coli
37AntibacterialActivity +e Pad-Dry-Cure treated fabricexhibited maximum antibacterial activity against Gram-negative test organisms compared to the Gram-positivetest organisms Maximum bacteria reduction was observedagainst Staphylococcus aureus and Escherichia coli whenthe padding mangle was applied at a pressure of 15 barwith 20 30 and 40 minutes of wetting time +is resultdemonstrated that the higher the wetting time (30 minutesand 40 minutes) in padding the better the antibacterialproperties At lower wetting time 20 minutes the anti-bacterial property is low as compared to the other wetting
Journal of Chemistry 5
Predicted vs actual
Color points by value ofyield25 55
30 35 40 504525 55Actual
25
30
35
40
45
50
55Pr
edic
ted
(a)
Color points by value ofyield29 59
Predicted vs actual
30 40 5020 60Actual
20
30
40
50
60
Pred
icte
d
(b)
Figure 2 Correlation between actual value and predicted value of (a) water and (b) ethanol extraction yield
Table 3 Analysis of variance (ANOVA) of the water extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 98997 2 49499 244408 lt00001
SignificantA time 79198 1 79198 391052 lt00001B conc 19799 1 19799 97763 lt00001Residual 203 10 02025Lack of fit 00253 6 00042 00084 10000 Not significantPure error 200 4 05000Cor total 99200 12
Table 4 Analysis of variance (ANOVA) of the ethanol extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 90780 2 45390 53341 lt00001
SignificantA time 70980 1 70980 83415 lt00001B conc 19799 1 19799 23268 lt00001Residual 851 10 08509Lack of fit 651 6 108 217 02367 Not significantPure error 200 4 05000Cor total 91631 12
Yield ()
Yiel
d (
)
55
50
45
40
35
30
25
25
20B concentration (mlg)
A time (m
inute)
1510 30
4050
6070
809030
Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
25 55
(a)
Yiel
d (
)
60
50
40
30
20
B concentration (mlg) A time (m
inute)25
2015
10 3040
5060
7080
9030
Yield ()Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
29 59
(b)
Figure 3 Interaction of factors time and temperature on (a) water and (b) ethanol extraction yield
Table 7 Optimization at minimum time concentration and high yield
Number Time (min) Conc(mlg) Yield () Desirability1 59896 10000 34991 0551 Selected
Table 8 Optimization at minimum time concentration and high yield
Number Time (min) Concentration (mlg) Yield Desirability1 59026 10458 38716 0547 Selected
008
006
004
002
000
4000 3500 3000 2500 2000Wave number (cmndash1)
1500 1000 500 0
Abso
rban
ce (
)
Untreated fabricTreated fabric dry
Powder extractedPowder
(a)
1000800600Temperature (degC)4002000
0
ndash5
ndash10
ndash15
ndash20
Mas
s los
s (m
g)
ndash25
ndash30
1200
(b)
Figure 4 Functional group and thermal analysis of nettle leaf extracted powder (a) combined FTIR spectra of untreated cotton fabric (b)thermography resulting from TGA analysis obtained under a nitrogen flow of 50mlmin and heating rate of 10degCmin
+
+
H
H C COOHH
H C C
O
O
OOC
HO C COOH
H
H
CHO
OH ndash celluloseCellulose
OH
RR R
R
RR
R
R
RR
C COOH
H
H
CCOOH
Citric acid Phenol derivatives
Figure 5 Mechanism of reaction between cellulose citric acid and phenolic compounds [48]
Journal of Chemistry 7
time +is effect could be becuase the longer the wettingtime of each particle of the extracted agents the deeper thepenetration inside the cotton fiber and the better thedurability (Table 9 Figure 6)
38 Durability to Laundering Generally the finishedscoured cotton fabric subjected to number of wash cycles (510 15 20 25 30 35 and 40) showed a gradual decrease inantibacterial property with 100 to 44 reduction in thebacterial count for Staphylococcus aureus and 100 to 30reduction in the bacterial count for Escherichia coli(Figure 7)
Citric acid as a crosslinking agent was added to theantibacterial finishing solutions It was found that the citric
acid was fairly effective against bacteria Adding poly-carboxylic acids to the antibacterial finishing recipes willenhance the durability of many laundering cycles
4 Conclusion
Natural and eco-friendly antibacterial finishing of textiles astrong antibacterial finishing of textile substrates withgood fastness and stability was obtained with nettle leafextract crosslinking on cotton fabrics using citric acid Itexhibits higher antibacterial efficiency +ere was a 100 to9975 percent reduction in the count of test bacteria afterPad-Dry-Cure treatment of the scoured cotton fabrics withthe dry nettle leaf extracted with optimized variables +eoptimization of the Pad-Dry-Cure conditions for finishing
S aureusSoaking time-20 minutes
S aureusSoaking time-30 minutes
S aureusSoaking time-40 minutes
E coliSoaking time-20 minutes
E coliSoaking time-30 minutes
E coliSoaking time-40 minutes
Figure 6 +e test results of Pad-Dry-Cure antibacterial treated fabric for Staphylococcus aureus and Escherichia coli
Aer 5 wash Aer 10 wash Aer 15 wash Aer 20 wash
Aer 25 wash Aer 30 wash Aer 35 wash Aer 40 wash
Figure 7 +e test results of wash durability for the treated fabrics (note A Escherichia coli B Staphylococcus aureus)
Table 9 Bacterial reduction test on the Pad-Dry-Cure treated fabric
was assessed for bacterial reduction test against Escherichiacoli and Staphylococcus aureus Maximum bacterial re-duction percentage was observed against Staphylococcusaureus and Escherichia coli when the wetting time was 30and 40minutes
Data Availability
+e authors have annotated the entire data building processthe empirical techniques presented in the paper and thenumber of runs generated using Design-Expert and Minitab18 software for optimization and analyzation based on theirparameters All data used to support the findings of thisstudy are included within the paper
Conflicts of Interest
Asnake Ketema is currently working as a lecturer in textilechemistry at Dire Dawa Institute of Technology Dire DawaUniversity Dire Dawa Ethiopia Amare Worku is cur-rently working as lecturer in textile chemistry and SchoolDean of the School of Textile Apparel and Fashion Designat Dire Dawa Institute of Technology Dire Dawa Uni-versity Dire Dawa Ethiopia +e authors declare that thereare no conflicts of interest regarding the publication of thispaper
Acknowledgments
+e authors would like to thank their advisor Dr GNalankilli professor of textile chemistry for his supportinvaluable guidance and constructive criticism during thesiswork and Dr Tamrat Tesfaye the secretary of the committeefor his encouragement and hard questions +is work wouldnot have been possible without the financial support of theEthiopian Institute of Textile and Fashion Technology(EiTEX) only for research work
References
[1] A Kalia B Joshi and M Mukhija ldquoPharmacognostical re-view of Urtica dioica Lrdquo International Journal of GreenPharmacy (IJGP) vol 8 no 4 pp 1998ndash4103 2014
[2] J Sheikh N Singh and M Srivastava ldquoFunctional dyeing ofcellulose-based (linen) fabric using Bombax ceiba (kapok)flower extractrdquo Fibers and Polymers vol 20 no 2 pp 312ndash319 2019
[3] L Qian ldquoApplication of nanotechnology for high perfor-mance textilesrdquo Journal of Textile and Apparel Technologyand Management vol 4 no 1 pp 1ndash7 2004
[4] C K Kang S S Kim S Kim et al ldquoAntibacterial cotton fiberstreated with silver nanoparticles and quaternary ammoniumsaltsrdquo Carbohydrate Polymers vol 151 pp 1012ndash1018 2016
[5] J E Herrera ldquoSynthesis of nanodispersed oxides of vanadiumtitanium molybdenum and tungsten on Mesoporous silicausing atomic layer depositionrdquo Topics in Catalysis vol 39no 3-4 pp 245ndash255 2006
[6] J Hudec M Burdova L u Kobida et al ldquoAntioxidant ca-pacity changes and phenolic profile of Echinacea purpureanettle (Urtica dioica L) and dandelion (Taraxacum officinale)after application of polyamine and phenolic biosynthesis
regulatorsrdquo Journal of Agricultural and Food Chemistryvol 55 no 14 pp 5689ndash5696 2007
[7] N A Ibrahim M H Abo-Shosha M A GaffarA M Elshafei and O M Abdel-Fatah ldquoAntibacterialproperties of ester-cross-linked cellulose-containing fabricspost-treated with metal saltsrdquo Polymer-Plastics Technologyand Engineering vol 45 no 6 pp 719ndash727 2006
[8] G +ilagavathi and S K Bala ldquoMicroencapsulation of herbalextracts for microbial resistance in healthcare textilesrdquoJournal of Fiber and Textile Research vol 32 no 1 pp 351ndash354 2007
[9] N A Salih ldquoAntibacterial effect of nettle (Urtica dioica)rdquo Al-Qadisiyah Journal of Veterinary Medicine Sciences vol 13no 1 p 1 2014
[10] K K Ghaima N M Hashim and S A Ali ldquoAntibacterial andantioxidant activities of ethyl acetate extract of nettle (Urticadioica) and dandelion (Taraxacum officinale)rdquo Journal ofApplied Pharmaceutical Science vol 3 no 5 p 96 2013
[11] T L Vigo Protection of Textiles from Biological AttackWoodhead Publishing Sawston UK 1st edition 2005
[12] S Hashemikia andMMontazer ldquoSodium hypophosphite andnano TiO2 inorganic catalysts along with citric acid on textileproducing multi-functional propertiesrdquo Applied Catalysis AGeneral vol 417-418 pp 200ndash208 2012
[13] M Montazer and M G Afjeh ldquoSimultaneous x-linking andantimicrobial finishing of cotton fabricrdquo Journal of AppliedPolymer Science vol 103 no 1 pp 178ndash185 2007
[14] R Aladpoosh and M Montazer ldquo+e role of cellulosic chainsof cotton in biosynthesis of ZnO nanorods producing mul-tifunctional properties mechanism characterizations andfeaturesrdquo Carbohydrate Polymers vol 126 pp 122ndash129 2015
[15] PS Vankar ldquoAntibacterial and antioxidant activities of ethylacetate extract of nettle (Urtica dioica) and dandelion (Tar-axacum officinale)rdquo Journal of Applied Pharmaceutical Sci-ence vol 3 pp 096ndash099 2013
[16] T Nithya J Jayanthi and M Ragunathan ldquoAntioxidantactivity total phenol flavonoid alkaloid tannin and saponincontents of leaf extracts of Salvinia molesta DS MitchellrdquoAsian Journal of Pharmaceutical and Clinical Research vol 9no 1 pp 200ndash203 2016
[17] R Roghini and K J Vijayalakshmi ldquoPhytochemical screen-ing quantitative analysis of flavonoids and minerals inethanolic extract of citrus paradisirdquo International Journal ofPharmaceutical Sciences and Research vol 9 no 11pp 4859ndash4864 2018
[18] F Sidaoui ldquoStudy of Tunisian nettle leaves (Urtica dioica L)mineral composition and antioxidant capacity of their ex-tracts obtained by maceration and supercritical fluid ex-tractionrdquo International Journal of Pharmacognosy andPhytochemical Research vol 7 pp 707ndash713 2015
[19] B Simoncic and B Tomsic ldquoStructures of novel antimicrobialagents for textiles-a reviewrdquo Textile Research Journal vol 80no 16 pp 1721ndash1737 2010
[20] G Sun and S D Worley ldquoChemistry of durable and re-generable biocidal textilesrdquo Journal of Chemical Educationvol 82 no 1 p 60 2005
[21] P Jaswal S AgyaPreet and G J Goel ldquoAntimicrobial activityof herbal treated cotton fabricrdquo International ResearchJournal of Engineering and Technology vol 4 no 8 pp 39ndash432017
[22] M Sathianarayanan ldquoAntibacterial finish for cotton fabricfrom herbal productsrdquo Indian Journal of Fiber and TextileResearch vol 35 pp 50ndash58 2010
Journal of Chemistry 9
[23] D Kut ldquoEffects of environmental conditions on the anti-bacterial activity of treated cotton knitsrdquo AATCC Reviewvol 5 no 3 2005
[24] N Afraz ldquoAntimicrobial finishes for textilesrdquo Including re-sults for Curr Trends Fashion Technology Textile Engineeringvol 5 p 4 2019
[25] A El-Shafei ldquoHerbal extract as an ecofriendly antibacterialfinishing of cotton fabricrdquo Egyptian Journal of Chemistryvol 61 no 2 pp 317ndash327 2018
[26] A Haji M Nasiriboroumand and S S Qavamnia ldquoCottondyeing and antibacterial finishing using agricultural waste byan eco-friendly process optimized by response surfacemethodologyrdquo Fibers and Polymers vol 19 no 11pp 2359ndash2364 2018
[27] A Reshma V B Priyadarisini and K Amutha ldquoSustainableantimicrobial finishing of fabrics using natural bioactiveagentsrdquo International Journal of Life Science vol 4 pp 10ndash202018
[28] W Ibrahim ldquoAloe vera leaf gel extract for antibacterial andsoftness properties of cottonrdquo Journal of Textile Science ampEngineering vol 7 no 301 p 2 2017
[29] P S Vankar R Shanker and S Wijayapala ldquoDyeing ofcotton wool and silk with extract of Allium cepardquo Pigment ampResin Technology vol 38 no 4 pp 242ndash247 2009
[30] G Singh ldquoFunctionalization of wool fabric using kapokflower and bio-mordantrdquo Sustainable Chemistry and Phar-macy vol 14 pp 2352ndash5541 2019
[31] K Gong Y Pan L J Rather et al ldquoNatural pigment duringflora leaf senescence and its application in dyeing and UVprotection finish of silk and woolmdasha case study of Cinna-momum camphorardquoDyes and Pigments vol 166 pp 114ndash1212019
[32] J Sheikh ldquoUltrasound assisted extraction of natural dyes andnatural mordants vis a vis dyeingrdquo Fibers and Polymersvol 17 no 5 pp 738ndash743 2016
[33] K Koszegi ldquoAntimicrobial Effects of the stinging nettle(Urtica dioica L)rdquo Analecta Technical Szegedinensia vol 11p 22 2017
[34] K Belay andM J C M R Sisay ldquoPhytochemical constituentsand physicochemical properties of medicinal plant (Moringaoleifera) around Bule Horardquo Chemistry and Materials Re-search vol 6 no 7 pp 61ndash72 2014
[35] K Murugesh Babu and K B Ravindra ldquoBioactive antimi-crobial agents for finishing of textiles for health care prod-uctsrdquo 4e Journal of the Textile Institute vol 106 no 7pp 706ndash717 2015
[36] I Gulccedilin ldquoAntioxidant antimicrobial antiulcer and analgesicactivities of nettle (Urtica dioica L)rdquo Journal of Ethno-pharmacology vol 90 no 2-3 pp 205ndash215 2004
[37] P Mantecca E Moschini P Bonfanti et al ldquoToxicity eval-uation of a new Zn-doped CuO nanocomposite with highlyeffective antibacterial propertiesrdquo Toxicological Sciencesvol 146 no 1 pp 16ndash30 2015
[38] V K Midha A Dakuri and V Midha ldquoStudies on theproperties of nonwoven surgical gownsrdquo Journal of IndustrialTextiles vol 43 no 2 pp 174ndash190 2013
[39] S W Ali S Rajendran and M Joshi ldquoSynthesis and char-acterization of chitosan and silver loaded chitosan nano-particles for bioactive polyesterrdquo Carbohydrate Polymersvol 83 no 2 pp 438ndash446 2011
[40] G M L Bearman A Rosato K Elam et al ldquoA crossover trialof antimicrobial scrubs to reduce methicillin-resistantStaphylococcus aureus burden on healthcare worker apparelrdquo
Infection Control amp Hospital Epidemiology vol 33 no 3pp 268ndash275 2012
[41] F Eser and A Onal ldquoDyeing of wool and cotton with extractof the nettle (Urtica dioica L) leavesrdquo Journal of NaturalFibers vol 12 no 3 pp 222ndash231 2015
[42] G Bag ldquoAssessment of total flavonoid content and antioxi-dant activity of methanolic rhizome extract of threeHedychium species of Manipur valleyrdquo International Journalof Pharmaceutical Sciences vol 30 no 1 pp 154ndash159 2015
[43] S ETHurovic ldquoChemical composition of stinging nettle leavesobtained by different analytical approachesrdquo Journal ofFunctional Food vol 32 pp 18ndash26 2017
[44] C S Ezeonu and C M Ejikeme ldquoQualitative and quantitativedetermination of phytochemical contents of indigenousNigerian softwoodsrdquo New Journal of Science vol 56 ArticleID 5601327 9 pages 2016
[45] H Y Fu S J Chen R F Chen W H Ding L L Kuo-Huangand R N Huang ldquoIdentification of oxalic acid and tartaricacid as major persistent pain-inducing toxins in the stinginghairs of the nettle Urtica thunbergianardquo Annals of Botanyvol 98 no 1 pp 57ndash65 2006
[46] Y Gao and R Cranston ldquoRecent advances in antimicrobialtreatments of textilesrdquo Textile Research Journal vol 78 no 1pp 60ndash72 2008
[47] S W Ali ldquoAntibacterial properties of aloe vera gel-finishedcotton fabricrdquo Cellulose vol 21 no 3 pp 2063ndash2072 2014
[48] M Gupta S +akur A Sharma and S Gupta ldquoQualitativeand quantitative analysis of phytochemicals and pharmaco-logical value of some dye yielding medicinal plantsrdquo OrientalJournal of Chemistry vol 29 no 2 pp 475ndash481 2013
10 Journal of Chemistry
advanced and innovative technologies are required Severalchemicals have been employed to impart antimicrobialactivity to textile goods +ose chemicals embrace inorganicsalts organ metallics iodophors (substances that slowlyrelease iodine) phenols and thiophenols antibiotics het-erocyclic and anionic groups and related compoundsformaldehyde derivatives and amines Many of thesechemicals however are toxic to humans they do not easilydegrade in the environment [9 10] Although chemicalantimicrobials are effective against a wide range of microbesthey are cause of concern due to the associated side effectsand water pollution +e use of synthetic products is be-coming increasingly problematic leading to microbial re-sistance product withdrawal undesirable environmentalproblems and animal toxicity [11ndash14] Hence there is agreat demand for antimicrobial treated textiles based on eco-friendly agents helping to effectively reduce the ill effectsassociated with microbial growth on textile material[11 15ndash20] +e use of natural plant products for antimi-crobial finishing of textile materials has been widely re-ported+ere are vast sources of medicinal plants with activeantimicrobial ingredients such as tulsi pomegranate andeucalyptus [21] +e research on their use in textiles is verylimited and not well documented+ese natural products areassociated with various benefits like lower incidence ofadverse reactions and reduced cost compared to syntheticpharmaceutical products and can be exploited as an at-tractive eco-friendly alternative to synthetic antimicrobialagents for textile applications [22 23]
Ginkgo-Biloba extract is an eco-friendly antimicrobialagent and its application was investigated in health andmedicinal purposes Due to its nontoxicity characteristics itis a potential candidate for antimicrobial finishing of in-stitutional textiles range including home accessories hos-pital bed sheets nursesrsquo uniforms and surgical gowns anddrapes+e plant-based natural fruit source was reported forits antimicrobial properties the fruit-based source is pine-apple (Ananas comosus) whose juice was investigated for itsactivity against harmful microbes +e antimicrobial activitywas evaluated through the agar diffusion method Anotherplant-based source reported is papaya (Carica papaya) [2425] Berberis vulgaris L wood as an agricultural waste wasused for dyeing and functional finishing of cotton To fa-cilitate the attachment of natural dye citric acid was used tocreate carboxylic acid functional groups on cotton fibers+e dyed sample prepared under the optimum conditions ofcrosslinking showed good wash and light fastness propertiesbesides very good antibacterial activity against Gram-neg-ative and Gram-positive bacteria [26]
+e chitosan and alginate have been used for antimi-crobial finishing of textiles Chitosan is a derivate of chitin itis water-soluble and cellulose-based Chitin is a polysac-charide based on amino sugars In an acid solvent the aminecomponent turns into a quarterly amino unit that inhibitsthe growth of microbes +is amino unit works as a shield toblock the protein and slow down proliferation by distractingcell membrane this permits the substance to escape from thebacterial cell resulting in the death of the bacteria Anti-microbial activity of chitosan was reported in many studies
and it is a widely accepted antimicrobial agent [8] Severalnatural agents such as basil (with active agent being euge-nol) neem (with active limonoids like azadirachtin nim-binin) turmeric (curcumin) clove oil chitosan sericinonion aloe vera and pomegranate have antimicrobialproperties [27 28]
Natural dye is now fast growing compared to syntheticdye for its safe healthy and eco-friendly nature and ap-plication Extraction and utilization of natural pigmentshave received broad attention in the current years Kapokflower is an unexplored source of natural dyestuff which canalso be utilized for the functionalization of cellulose-basedtextiles [29] Kapok flower extract (KFC) was utilized as afunctional dye for dyeing of linen fabric in the presence ofmetallic mordants +e dyed fabrics were assessed for col-oration properties (color values color coordinates andfastness properties) as well as functional properties such asantibacterial activity UV protection and antioxidant ac-tivity +e dyed fabrics displayed an excellent antibacterialactivity against Gram-positive and Gram-negative bacteria[2]
+e coloration of wool by kapok flower extract (KFE) bytannin-based natural mordant using premordanting treatingtechnique could impart important functional properties tothe dyed fabrics Wool fabrics were mordanted usingtamarind seed coats extract (TSCE) and further dyed withKFE +e dyed fabrics were evaluated for coloration prop-erties (color values fastness properties) as well as functionalproperties like antibacterial and antioxidant activity [30]Flora forest is a major component that contributes to thenatural resources from which natural pigment can be de-rived Both silk and wool showed excellent dyeing abilitywhen dyed with the extracted pigments Fabrics dyed withleaf pigments showed an unchanged or increased color-fastness to light washing and storage +is is because therich content of phenolic hydroxyl within leaf chemicalstructure is sensitive to light and alkaline condition and canresult in a hyperchromic effect [31] +e natural dyes requiremordants for their fixation on textile materials Naturalmordants are thus gaining importance in order to getcomplete-natural dyeing +e natural mordants namelyhard and tamarind seed coat and natural dyes like turmericand henna were extracted using conventional and ultra-sound approaches and various extracts obtained were de-scribed in terms of their optical densities +e combinationsof mordantsdyes and dyed fabrics were evaluated for theircolor strength and fastness properties [32]
Stinging nettle (Urtica dioica L) is grown in many areasacross the world annually It belongs to medicinal herbs [33]Several findings show that the stinging nettle (Urtica dioicaL) plant contains compounds like alkaloids phenols sa-ponins steroids tannins and glycosides which exhibit an-timicrobial properties [15] +e leaf extracts of nettle (Urticadioica) were studied and reported to have excellent anti-microbial activity against microorganisms based on theavailability of large amounts of bioactive compounds such astannins flavonoids and alkaloids which are effective againstbacterial and fungal infections [9] With respect to that theuse of nettle (Urtica dioica) leaf extract as a textile finish on
2 Journal of Chemistry
cotton fabrics has not been examined and reported in anyform
In the current study the interaction of extracted com-ponents from the nettle plant leaf with cotton fabric usingcitric acid and their potential antimicrobial efficacy againstStaphylococcus aureus and Escherichia coli bacterial specieswhich are known to cause cross infections in the cottonfabric as well as being responsible for causing unpleasantodors in textiles were investigated
2 Materials and Methods
21 Materials and Apparatus Citric acid was used as aprecursor for the crosslinking agent between extractedpowder and fabric Ethanol (CH3CH2OH 97 purity) wasprepared according to the procedure needed for the ex-traction of chemical ingredients from the nettle leaf
A hundred percent of scoured cotton fabric was used inthis study to ensure complete wetting and uniform absor-bency of the solution during padding Scouring treatmentwas applied to the woven cotton fabric to remove foreignmaterial before imparting antibacterial finish
+e following apparatus was used in this study ultra-sonic extractor electronic balance oven dryer Whatmanfilter paper No 1 pHmeter measuring cylinder Condensermagnetic stirrer crucible muffle furnace FTIR TGA UVspectroscopy and padding mangle
22 Preparation of Sample +e plant leaf was collected fromAmhara region in Debre Tabor Ethiopia and washed withpure water rinsed with distilled water cleaned air-dried for8 days and cut into small pieces for further size reductioninto fine powder with the help of electric grinder up to0710 μm particle size Major phenolic chemical ingredientsof nettle leaf extract are given in Figure 1
23 Ultrasonic Extraction Technique Ultrasonic assistedextraction (UAE) method has been considered according toits simplicity to extract the responsible chemical com-pounds easy handling low cost high yield or efficiencylower organic extraction solvent consumption reduced timefor extraction and reliable procedure in an extensive rangeof organic solvents for various phenolic compounds in large-scale level and industry Air-dried nettle leaf sample 20grams was prepared in 200ml 400ml and 600ml of waterand 975 ethanol and extracted using ultrasonic extractiontechniques for 30 60 and 90 extraction minutes at 45ndash50degC(Table 1) +e extracted ingredient was filtered through afilter paper (Whatman No 1) which was impregnated withthe same solvents +e ethanol was concentrated to neardryness under reduced pressure below 50degC using a rotaryevaporator machine +e amount of the concentrated in-gredient extracted was noted down and stored in air tightglass bottles in a refrigerator until further use [35]
Based on the parameters in Table 2 antibacterial agentwas extracted and the number of trials is designed andgenerated using central composite design (CCD) Design-Expertreg version 11 software
24 Quantitative Phytochemical Analysis +e leaf extractthat exhibited the maximum antibacterial activity wasassessed for the presence of phytochemicals A preliminaryphytochemical analysis was performed to determine theamount of phenolic and flavonoid compounds in milligramper gram of extracted powder [36ndash38]
25 Determination of Total Phenolic Content (TPC)UV-spectrophotometric methods are most commonly usedfor the quantification of phenolic content Preparation ofstandard gallic acid solution was as follows 02 gram of gallicacid was dissolved into 200ml distilled water so the con-centration of the solution was 0001 gramml or 1000 microgml+is is called the stock solution +en serial dilution wasperformed in order to prepare different concentrations ofthe solution (0 gml 50 gml 100mgml 150mgml200mgml 250mgml and 300mgml) which are used forpreparing calibration curve
Estimation of total phenol content in the selected plantextract was measured spectrophotometrically byFolinndashCiocalteu (FCR) colorimetric method using gallicacid as the standard and expressing results as gallic acidequivalent (GAE) per gram of sample Different concen-trations (001mgml) of gallic acid were prepared inmethanol Aliquots of 1ml of the test sample and eachsample of the standard solution were taken and mixed with2ml of FolinndashCiocalteu reagent (1 10 in deionized water)and 4ml of a saturated solution of sodium carbonate (75wv) +e tubes were covered with silver foils and incubatedat room temperature for 30 minutes with intermittentshaking +e absorbance was taken at 765 nm using meth-anol as blank All the samples were analyzed in three rep-lications +e total phenolic amount was determined withthe help of a standard cure prepared from a pure phenolicstandard (gallic acid) [10 39 40]
TPCmgGAE
m1113874 1113875
ClowastV
m (1)
A formula was used to assess the phenolic compoundsin mg from one gram of extracted powder when the TPCamount increases the antibacterial activity will be effective
Here TPC is the total phenol content in mg of gallic acidequivalent per gram of extracted gallic acid equivalent m isdry mass of a sample in gram used for characterization C is aconcentration of gallic acid in mgl and V is the volume ofsample taken in a milliliter
26 Determination of Total Flavonoid Content (TFC) +eTFC of the leaf extract was determined by aluminumchloride colorimetric assay Briefly 05ml aliquots of theextract and standard solution (001ndash10mgml) of quercetinwere added to 2ml of distilled water and subsequently to015ml of sodium nitrite (5 NaNO2 wv) solution andmixed After 6 minutes 015ml of (10 AlCl3 wv) solutionwas added+e solutions were allowed to stand for quercetin6min and after that 2ml of sodium hydroxide (4 NaOHwv) solution was added to the mixture +e final volumewas adjusted to 5ml with immediate addition of distilled
Journal of Chemistry 3
water mixed thoroughly and allowed to stand for another15min +e absorbance of each mixture was determined at510 nm against the samemixture but without leaf extract as ablank TFC was determined as mg quercetin equivalent pergram of sample with the help of the calibration curve ofquercetin All measurements were performed in triplicate(n 3) [41]
TFCmgQUE
m1113874 1113875
ClowastV
m (2)
+e total flavonoid content of the extracts can be de-termined using the above formula where C is the concen-tration of quercetin in mgL of quercetin equivalence V isthe volume of sample taken (ml) m is the dry weight of
sample (g) and TFC is the total flavonoid content in mg ofquercetin equivalence
27 Functional Group and 4ermal Analysis FourierTransform Infrared (FTIR) Spectrophotometer is the mostpowerful tool for identifying the types of functional groupsbased on the wavelength of light absorbed By interpretingthe infrared absorption spectrum the chemical bonds in amolecule were determined [42]
+e TGA curve was obtained with a heating rate of10degCminminus1 in the temperature range of 30 to 1000degC byusing alumina crucibles and samplesrsquo mass of about 10mg+e experiments were carried out under the nitrogen at-mosphere at a flow rate of 50mlminminus1
28 Application Procedure Pad-Dry-Cure is most widelyused for 100 scoured cotton fabric Nettle leaf extractedpowder was treated with nine percent on weight of fabric(owf) under room temperature +e treated fabric waspassed between the rollers two to three times at a uniformpressure at 15 bar for better penetration of finishing agentand to squeeze out excess liquid from the fabric +e fabricwas then dried at 110degC and cured at 130degC in a curingchamber within 3 minutes
29 Antibacterial Test Antibacterial testing was done byAATCC standard test method 1002004 for the quantitativevaluation of the antibacterial effectiveness of the antimi-crobial agents against Gram-positive bacteria (Staphylo-coccus aureus) and Gram-negative bacteria (Escherichiacoli) Assessment of the percent reduction of bacteria wascalculated using
R() B minus A
B1113874 1113875 times 100 (3)
R is the percent reduction of bacteria A is the thenumber of bacteria recovered from the inoculated treatedtest specimen swatches in the jar incubated over the desiredcontact period B is the the number of bacteria recoveredfrom the inoculated untreated test specimen swatches in thejar incubated over the desired contact period microbes anddyed fabric
HO
HO
OH
OH
O
O
O
O
(a)
HO
HOHO
HO
OH
OH
OH
OH
H3C
OH
OH
O
OO
O
O
O
(b)
Figure 1 Chemical structures of extracted phenolic compound (a) 2-O-caffeoylmalic acid (b) rutin [33 34]
Table 1 Antibacterial agent extraction parameters water andethanol used as extraction solvents
Extraction factors ParametersMaterial to liquor ratio 1 10 1 20 1 30Extraction time (minutes) 30 60 90Extraction temperature (degC) 45ndash50
Table 2 Number of runs by using central composite design (CCD)and their yield
210 Wash Durability Test +e treated fabrics were laun-dered using AATCC test method 61 Laundering was carriedout at MLR of 1 10 with 05 on weight of fabric of AATCCdetergent and 100 steel balls at a temperature of 90degC for 30minutes +e washing cycle was followed by hot rinsing inplain water at 40degC for 10 minutes Finally the washedswatches were tumble-dried Since a single wash-dry cyclesimulated 8 regular wash cycles the laundering procedurewas repeated 5 10 15 20 25 30 35 and 40 times to checkchemical durability
3 Results and Discussion
31 Yield of Extraction Using Water and Ethanol +e ex-perimental results (Table 2) can be illustrated by the fol-lowing linear equation
Yield 1015076 + 033 time + 0497487 conc (4)
Yield 1498065 + 031 Time + 0497487Conc (5)
Equations (4) and (5) depict the yield that has a linearrelationship with the factor of extraction time and con-centration of water and ethanol used as extraction solventrespectively
+e actual value and model prediction value of the yieldshowed a good correlation (Figure 2) Based on the ANOVAanalysis the linear equation has a p-value of 00001 (lt005)indicating that the equation model is significant
32 Analysis of Variance (ANOVA) +e results of theANOVA analysis factors A and B had a significant effect(Tables 3 and 4) +e factors A and B had a p-value of 00001and 00001 respectively +e model showed that the factorsA and B had a positive effect on the extraction yield indi-cating an increase in these factors extraction yield increases(Figure 3)
33 Optimization Extraction Parameters +e optimumconditions are based on the resulting desirability value +egoal of extraction is to minimize extraction time concen-tration and maximum water and ethanol extraction yield asshown in Tables 5 and 6 respectively +e optimizationprocess was performed by establishing the highest level ofextraction yield
Table 7 shows that the optimal extraction time is 59minutes with concentration of 10mlg the predictiveyield is 34991 percent Ethanolic extraction yield hasoptimal extraction time of 59026 minute with concen-tration of 10458mlg the predictive yield is 38716percent (Table 8)
34 Quantitative Analysis of Phytochemical Ingredients+e amount of total phenol content in the extract was de-termined by the Folin-Ciocalteau reagent described in theMaterials and Methods section using gallic acid as thestandard +e absorbance values obtained at differentconcentrations of gallic acid were used for the construction
of a calibration curve It appeared that the extraction ofnettle plant leaf total phenolic content is 27819plusmn 0131mgGAEg dry weight (equation (1))+e total flavonoid contentin the extract of nettle plant leaves is 2566plusmn 0227mgGAEgdry weight (equation (2)) [43ndash46]
FTIR studied in extracted nettle leaf displayed strongabsorption peaks at 307819 cmminus1 154929 cmminus1 140509 cmminus1and 107781 cmminus1 +e broad peak between 3500 cmminus1 and2500 cmminus1 corresponds to a strong O-H stretch vibrationwhich indicates the presence of hydroxyl groups in nettle leafextract On finger print region a doublet band is presentbetween1390 cmminus1 and 1310 cmminus1 representing O-H bendingwhich indicates phenolic compounds +e FTIR spectra of thetreated and untreated cotton fabric were almost the same andslight differences were at wave number 3000ndash2500 cmminus1 +etreated fabric has O-H stretch vibration and OH functionalgroup between 3000 and 2500 cmminus1 (Figure 4(a))
+e TGA curves of the crude extract showed that asmall weight loss was found in the range of 90ndash162degC dueto the evaporation of the humidity of the materials orvolatile compounds 162ndash537degC was associated with ali-phatic phenolic compounds decomposition or degrada-tion Char formation was detected between 537 and1028degC by further extending the analysis temperature(Figure 4(b))
35 Effect of Tensile Strength +e tensile strength of the Pad-Dry-Cure treated cotton fabric decreased by 066 and 117percent compared to the untreated control in warp and weftdirection respectively
Other physical properties such as permeability stiffnessstrength and absorbency were tested accordingly based onASTM ISO and AATCC standard respectively [33 47]
36 ReactionMechanisms +e two carboxylic groups of thecitric acid are linked with the hydroxyl part of the celluloseand with extracted phenol through covalent bond (Figure 5)+eir effective antibacterial activity and phenolic com-pounds were attached to cotton fabric using citric acid as acrosslinker Phenolic compounds are among the major anddiverse groups of active compounds in the nettle plant leafCotton fabrics treated with phenolic compounds showedexcellent antibacterial activity against the Gram-positivebacteria Staphylococcus aureus as well as the Gram-negativebacteria Escherichia coli
37AntibacterialActivity +e Pad-Dry-Cure treated fabricexhibited maximum antibacterial activity against Gram-negative test organisms compared to the Gram-positivetest organisms Maximum bacteria reduction was observedagainst Staphylococcus aureus and Escherichia coli whenthe padding mangle was applied at a pressure of 15 barwith 20 30 and 40 minutes of wetting time +is resultdemonstrated that the higher the wetting time (30 minutesand 40 minutes) in padding the better the antibacterialproperties At lower wetting time 20 minutes the anti-bacterial property is low as compared to the other wetting
Journal of Chemistry 5
Predicted vs actual
Color points by value ofyield25 55
30 35 40 504525 55Actual
25
30
35
40
45
50
55Pr
edic
ted
(a)
Color points by value ofyield29 59
Predicted vs actual
30 40 5020 60Actual
20
30
40
50
60
Pred
icte
d
(b)
Figure 2 Correlation between actual value and predicted value of (a) water and (b) ethanol extraction yield
Table 3 Analysis of variance (ANOVA) of the water extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 98997 2 49499 244408 lt00001
SignificantA time 79198 1 79198 391052 lt00001B conc 19799 1 19799 97763 lt00001Residual 203 10 02025Lack of fit 00253 6 00042 00084 10000 Not significantPure error 200 4 05000Cor total 99200 12
Table 4 Analysis of variance (ANOVA) of the ethanol extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 90780 2 45390 53341 lt00001
SignificantA time 70980 1 70980 83415 lt00001B conc 19799 1 19799 23268 lt00001Residual 851 10 08509Lack of fit 651 6 108 217 02367 Not significantPure error 200 4 05000Cor total 91631 12
Yield ()
Yiel
d (
)
55
50
45
40
35
30
25
25
20B concentration (mlg)
A time (m
inute)
1510 30
4050
6070
809030
Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
25 55
(a)
Yiel
d (
)
60
50
40
30
20
B concentration (mlg) A time (m
inute)25
2015
10 3040
5060
7080
9030
Yield ()Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
29 59
(b)
Figure 3 Interaction of factors time and temperature on (a) water and (b) ethanol extraction yield
Table 7 Optimization at minimum time concentration and high yield
Number Time (min) Conc(mlg) Yield () Desirability1 59896 10000 34991 0551 Selected
Table 8 Optimization at minimum time concentration and high yield
Number Time (min) Concentration (mlg) Yield Desirability1 59026 10458 38716 0547 Selected
008
006
004
002
000
4000 3500 3000 2500 2000Wave number (cmndash1)
1500 1000 500 0
Abso
rban
ce (
)
Untreated fabricTreated fabric dry
Powder extractedPowder
(a)
1000800600Temperature (degC)4002000
0
ndash5
ndash10
ndash15
ndash20
Mas
s los
s (m
g)
ndash25
ndash30
1200
(b)
Figure 4 Functional group and thermal analysis of nettle leaf extracted powder (a) combined FTIR spectra of untreated cotton fabric (b)thermography resulting from TGA analysis obtained under a nitrogen flow of 50mlmin and heating rate of 10degCmin
+
+
H
H C COOHH
H C C
O
O
OOC
HO C COOH
H
H
CHO
OH ndash celluloseCellulose
OH
RR R
R
RR
R
R
RR
C COOH
H
H
CCOOH
Citric acid Phenol derivatives
Figure 5 Mechanism of reaction between cellulose citric acid and phenolic compounds [48]
Journal of Chemistry 7
time +is effect could be becuase the longer the wettingtime of each particle of the extracted agents the deeper thepenetration inside the cotton fiber and the better thedurability (Table 9 Figure 6)
38 Durability to Laundering Generally the finishedscoured cotton fabric subjected to number of wash cycles (510 15 20 25 30 35 and 40) showed a gradual decrease inantibacterial property with 100 to 44 reduction in thebacterial count for Staphylococcus aureus and 100 to 30reduction in the bacterial count for Escherichia coli(Figure 7)
Citric acid as a crosslinking agent was added to theantibacterial finishing solutions It was found that the citric
acid was fairly effective against bacteria Adding poly-carboxylic acids to the antibacterial finishing recipes willenhance the durability of many laundering cycles
4 Conclusion
Natural and eco-friendly antibacterial finishing of textiles astrong antibacterial finishing of textile substrates withgood fastness and stability was obtained with nettle leafextract crosslinking on cotton fabrics using citric acid Itexhibits higher antibacterial efficiency +ere was a 100 to9975 percent reduction in the count of test bacteria afterPad-Dry-Cure treatment of the scoured cotton fabrics withthe dry nettle leaf extracted with optimized variables +eoptimization of the Pad-Dry-Cure conditions for finishing
S aureusSoaking time-20 minutes
S aureusSoaking time-30 minutes
S aureusSoaking time-40 minutes
E coliSoaking time-20 minutes
E coliSoaking time-30 minutes
E coliSoaking time-40 minutes
Figure 6 +e test results of Pad-Dry-Cure antibacterial treated fabric for Staphylococcus aureus and Escherichia coli
Aer 5 wash Aer 10 wash Aer 15 wash Aer 20 wash
Aer 25 wash Aer 30 wash Aer 35 wash Aer 40 wash
Figure 7 +e test results of wash durability for the treated fabrics (note A Escherichia coli B Staphylococcus aureus)
Table 9 Bacterial reduction test on the Pad-Dry-Cure treated fabric
was assessed for bacterial reduction test against Escherichiacoli and Staphylococcus aureus Maximum bacterial re-duction percentage was observed against Staphylococcusaureus and Escherichia coli when the wetting time was 30and 40minutes
Data Availability
+e authors have annotated the entire data building processthe empirical techniques presented in the paper and thenumber of runs generated using Design-Expert and Minitab18 software for optimization and analyzation based on theirparameters All data used to support the findings of thisstudy are included within the paper
Conflicts of Interest
Asnake Ketema is currently working as a lecturer in textilechemistry at Dire Dawa Institute of Technology Dire DawaUniversity Dire Dawa Ethiopia Amare Worku is cur-rently working as lecturer in textile chemistry and SchoolDean of the School of Textile Apparel and Fashion Designat Dire Dawa Institute of Technology Dire Dawa Uni-versity Dire Dawa Ethiopia +e authors declare that thereare no conflicts of interest regarding the publication of thispaper
Acknowledgments
+e authors would like to thank their advisor Dr GNalankilli professor of textile chemistry for his supportinvaluable guidance and constructive criticism during thesiswork and Dr Tamrat Tesfaye the secretary of the committeefor his encouragement and hard questions +is work wouldnot have been possible without the financial support of theEthiopian Institute of Textile and Fashion Technology(EiTEX) only for research work
References
[1] A Kalia B Joshi and M Mukhija ldquoPharmacognostical re-view of Urtica dioica Lrdquo International Journal of GreenPharmacy (IJGP) vol 8 no 4 pp 1998ndash4103 2014
[2] J Sheikh N Singh and M Srivastava ldquoFunctional dyeing ofcellulose-based (linen) fabric using Bombax ceiba (kapok)flower extractrdquo Fibers and Polymers vol 20 no 2 pp 312ndash319 2019
[3] L Qian ldquoApplication of nanotechnology for high perfor-mance textilesrdquo Journal of Textile and Apparel Technologyand Management vol 4 no 1 pp 1ndash7 2004
[4] C K Kang S S Kim S Kim et al ldquoAntibacterial cotton fiberstreated with silver nanoparticles and quaternary ammoniumsaltsrdquo Carbohydrate Polymers vol 151 pp 1012ndash1018 2016
[5] J E Herrera ldquoSynthesis of nanodispersed oxides of vanadiumtitanium molybdenum and tungsten on Mesoporous silicausing atomic layer depositionrdquo Topics in Catalysis vol 39no 3-4 pp 245ndash255 2006
[6] J Hudec M Burdova L u Kobida et al ldquoAntioxidant ca-pacity changes and phenolic profile of Echinacea purpureanettle (Urtica dioica L) and dandelion (Taraxacum officinale)after application of polyamine and phenolic biosynthesis
regulatorsrdquo Journal of Agricultural and Food Chemistryvol 55 no 14 pp 5689ndash5696 2007
[7] N A Ibrahim M H Abo-Shosha M A GaffarA M Elshafei and O M Abdel-Fatah ldquoAntibacterialproperties of ester-cross-linked cellulose-containing fabricspost-treated with metal saltsrdquo Polymer-Plastics Technologyand Engineering vol 45 no 6 pp 719ndash727 2006
[8] G +ilagavathi and S K Bala ldquoMicroencapsulation of herbalextracts for microbial resistance in healthcare textilesrdquoJournal of Fiber and Textile Research vol 32 no 1 pp 351ndash354 2007
[9] N A Salih ldquoAntibacterial effect of nettle (Urtica dioica)rdquo Al-Qadisiyah Journal of Veterinary Medicine Sciences vol 13no 1 p 1 2014
[10] K K Ghaima N M Hashim and S A Ali ldquoAntibacterial andantioxidant activities of ethyl acetate extract of nettle (Urticadioica) and dandelion (Taraxacum officinale)rdquo Journal ofApplied Pharmaceutical Science vol 3 no 5 p 96 2013
[11] T L Vigo Protection of Textiles from Biological AttackWoodhead Publishing Sawston UK 1st edition 2005
[12] S Hashemikia andMMontazer ldquoSodium hypophosphite andnano TiO2 inorganic catalysts along with citric acid on textileproducing multi-functional propertiesrdquo Applied Catalysis AGeneral vol 417-418 pp 200ndash208 2012
[13] M Montazer and M G Afjeh ldquoSimultaneous x-linking andantimicrobial finishing of cotton fabricrdquo Journal of AppliedPolymer Science vol 103 no 1 pp 178ndash185 2007
[14] R Aladpoosh and M Montazer ldquo+e role of cellulosic chainsof cotton in biosynthesis of ZnO nanorods producing mul-tifunctional properties mechanism characterizations andfeaturesrdquo Carbohydrate Polymers vol 126 pp 122ndash129 2015
[15] PS Vankar ldquoAntibacterial and antioxidant activities of ethylacetate extract of nettle (Urtica dioica) and dandelion (Tar-axacum officinale)rdquo Journal of Applied Pharmaceutical Sci-ence vol 3 pp 096ndash099 2013
[16] T Nithya J Jayanthi and M Ragunathan ldquoAntioxidantactivity total phenol flavonoid alkaloid tannin and saponincontents of leaf extracts of Salvinia molesta DS MitchellrdquoAsian Journal of Pharmaceutical and Clinical Research vol 9no 1 pp 200ndash203 2016
[17] R Roghini and K J Vijayalakshmi ldquoPhytochemical screen-ing quantitative analysis of flavonoids and minerals inethanolic extract of citrus paradisirdquo International Journal ofPharmaceutical Sciences and Research vol 9 no 11pp 4859ndash4864 2018
[18] F Sidaoui ldquoStudy of Tunisian nettle leaves (Urtica dioica L)mineral composition and antioxidant capacity of their ex-tracts obtained by maceration and supercritical fluid ex-tractionrdquo International Journal of Pharmacognosy andPhytochemical Research vol 7 pp 707ndash713 2015
[19] B Simoncic and B Tomsic ldquoStructures of novel antimicrobialagents for textiles-a reviewrdquo Textile Research Journal vol 80no 16 pp 1721ndash1737 2010
[20] G Sun and S D Worley ldquoChemistry of durable and re-generable biocidal textilesrdquo Journal of Chemical Educationvol 82 no 1 p 60 2005
[21] P Jaswal S AgyaPreet and G J Goel ldquoAntimicrobial activityof herbal treated cotton fabricrdquo International ResearchJournal of Engineering and Technology vol 4 no 8 pp 39ndash432017
[22] M Sathianarayanan ldquoAntibacterial finish for cotton fabricfrom herbal productsrdquo Indian Journal of Fiber and TextileResearch vol 35 pp 50ndash58 2010
Journal of Chemistry 9
[23] D Kut ldquoEffects of environmental conditions on the anti-bacterial activity of treated cotton knitsrdquo AATCC Reviewvol 5 no 3 2005
[24] N Afraz ldquoAntimicrobial finishes for textilesrdquo Including re-sults for Curr Trends Fashion Technology Textile Engineeringvol 5 p 4 2019
[25] A El-Shafei ldquoHerbal extract as an ecofriendly antibacterialfinishing of cotton fabricrdquo Egyptian Journal of Chemistryvol 61 no 2 pp 317ndash327 2018
[26] A Haji M Nasiriboroumand and S S Qavamnia ldquoCottondyeing and antibacterial finishing using agricultural waste byan eco-friendly process optimized by response surfacemethodologyrdquo Fibers and Polymers vol 19 no 11pp 2359ndash2364 2018
[27] A Reshma V B Priyadarisini and K Amutha ldquoSustainableantimicrobial finishing of fabrics using natural bioactiveagentsrdquo International Journal of Life Science vol 4 pp 10ndash202018
[28] W Ibrahim ldquoAloe vera leaf gel extract for antibacterial andsoftness properties of cottonrdquo Journal of Textile Science ampEngineering vol 7 no 301 p 2 2017
[29] P S Vankar R Shanker and S Wijayapala ldquoDyeing ofcotton wool and silk with extract of Allium cepardquo Pigment ampResin Technology vol 38 no 4 pp 242ndash247 2009
[30] G Singh ldquoFunctionalization of wool fabric using kapokflower and bio-mordantrdquo Sustainable Chemistry and Phar-macy vol 14 pp 2352ndash5541 2019
[31] K Gong Y Pan L J Rather et al ldquoNatural pigment duringflora leaf senescence and its application in dyeing and UVprotection finish of silk and woolmdasha case study of Cinna-momum camphorardquoDyes and Pigments vol 166 pp 114ndash1212019
[32] J Sheikh ldquoUltrasound assisted extraction of natural dyes andnatural mordants vis a vis dyeingrdquo Fibers and Polymersvol 17 no 5 pp 738ndash743 2016
[33] K Koszegi ldquoAntimicrobial Effects of the stinging nettle(Urtica dioica L)rdquo Analecta Technical Szegedinensia vol 11p 22 2017
[34] K Belay andM J C M R Sisay ldquoPhytochemical constituentsand physicochemical properties of medicinal plant (Moringaoleifera) around Bule Horardquo Chemistry and Materials Re-search vol 6 no 7 pp 61ndash72 2014
[35] K Murugesh Babu and K B Ravindra ldquoBioactive antimi-crobial agents for finishing of textiles for health care prod-uctsrdquo 4e Journal of the Textile Institute vol 106 no 7pp 706ndash717 2015
[36] I Gulccedilin ldquoAntioxidant antimicrobial antiulcer and analgesicactivities of nettle (Urtica dioica L)rdquo Journal of Ethno-pharmacology vol 90 no 2-3 pp 205ndash215 2004
[37] P Mantecca E Moschini P Bonfanti et al ldquoToxicity eval-uation of a new Zn-doped CuO nanocomposite with highlyeffective antibacterial propertiesrdquo Toxicological Sciencesvol 146 no 1 pp 16ndash30 2015
[38] V K Midha A Dakuri and V Midha ldquoStudies on theproperties of nonwoven surgical gownsrdquo Journal of IndustrialTextiles vol 43 no 2 pp 174ndash190 2013
[39] S W Ali S Rajendran and M Joshi ldquoSynthesis and char-acterization of chitosan and silver loaded chitosan nano-particles for bioactive polyesterrdquo Carbohydrate Polymersvol 83 no 2 pp 438ndash446 2011
[40] G M L Bearman A Rosato K Elam et al ldquoA crossover trialof antimicrobial scrubs to reduce methicillin-resistantStaphylococcus aureus burden on healthcare worker apparelrdquo
Infection Control amp Hospital Epidemiology vol 33 no 3pp 268ndash275 2012
[41] F Eser and A Onal ldquoDyeing of wool and cotton with extractof the nettle (Urtica dioica L) leavesrdquo Journal of NaturalFibers vol 12 no 3 pp 222ndash231 2015
[42] G Bag ldquoAssessment of total flavonoid content and antioxi-dant activity of methanolic rhizome extract of threeHedychium species of Manipur valleyrdquo International Journalof Pharmaceutical Sciences vol 30 no 1 pp 154ndash159 2015
[43] S ETHurovic ldquoChemical composition of stinging nettle leavesobtained by different analytical approachesrdquo Journal ofFunctional Food vol 32 pp 18ndash26 2017
[44] C S Ezeonu and C M Ejikeme ldquoQualitative and quantitativedetermination of phytochemical contents of indigenousNigerian softwoodsrdquo New Journal of Science vol 56 ArticleID 5601327 9 pages 2016
[45] H Y Fu S J Chen R F Chen W H Ding L L Kuo-Huangand R N Huang ldquoIdentification of oxalic acid and tartaricacid as major persistent pain-inducing toxins in the stinginghairs of the nettle Urtica thunbergianardquo Annals of Botanyvol 98 no 1 pp 57ndash65 2006
[46] Y Gao and R Cranston ldquoRecent advances in antimicrobialtreatments of textilesrdquo Textile Research Journal vol 78 no 1pp 60ndash72 2008
[47] S W Ali ldquoAntibacterial properties of aloe vera gel-finishedcotton fabricrdquo Cellulose vol 21 no 3 pp 2063ndash2072 2014
[48] M Gupta S +akur A Sharma and S Gupta ldquoQualitativeand quantitative analysis of phytochemicals and pharmaco-logical value of some dye yielding medicinal plantsrdquo OrientalJournal of Chemistry vol 29 no 2 pp 475ndash481 2013
10 Journal of Chemistry
cotton fabrics has not been examined and reported in anyform
In the current study the interaction of extracted com-ponents from the nettle plant leaf with cotton fabric usingcitric acid and their potential antimicrobial efficacy againstStaphylococcus aureus and Escherichia coli bacterial specieswhich are known to cause cross infections in the cottonfabric as well as being responsible for causing unpleasantodors in textiles were investigated
2 Materials and Methods
21 Materials and Apparatus Citric acid was used as aprecursor for the crosslinking agent between extractedpowder and fabric Ethanol (CH3CH2OH 97 purity) wasprepared according to the procedure needed for the ex-traction of chemical ingredients from the nettle leaf
A hundred percent of scoured cotton fabric was used inthis study to ensure complete wetting and uniform absor-bency of the solution during padding Scouring treatmentwas applied to the woven cotton fabric to remove foreignmaterial before imparting antibacterial finish
+e following apparatus was used in this study ultra-sonic extractor electronic balance oven dryer Whatmanfilter paper No 1 pHmeter measuring cylinder Condensermagnetic stirrer crucible muffle furnace FTIR TGA UVspectroscopy and padding mangle
22 Preparation of Sample +e plant leaf was collected fromAmhara region in Debre Tabor Ethiopia and washed withpure water rinsed with distilled water cleaned air-dried for8 days and cut into small pieces for further size reductioninto fine powder with the help of electric grinder up to0710 μm particle size Major phenolic chemical ingredientsof nettle leaf extract are given in Figure 1
23 Ultrasonic Extraction Technique Ultrasonic assistedextraction (UAE) method has been considered according toits simplicity to extract the responsible chemical com-pounds easy handling low cost high yield or efficiencylower organic extraction solvent consumption reduced timefor extraction and reliable procedure in an extensive rangeof organic solvents for various phenolic compounds in large-scale level and industry Air-dried nettle leaf sample 20grams was prepared in 200ml 400ml and 600ml of waterand 975 ethanol and extracted using ultrasonic extractiontechniques for 30 60 and 90 extraction minutes at 45ndash50degC(Table 1) +e extracted ingredient was filtered through afilter paper (Whatman No 1) which was impregnated withthe same solvents +e ethanol was concentrated to neardryness under reduced pressure below 50degC using a rotaryevaporator machine +e amount of the concentrated in-gredient extracted was noted down and stored in air tightglass bottles in a refrigerator until further use [35]
Based on the parameters in Table 2 antibacterial agentwas extracted and the number of trials is designed andgenerated using central composite design (CCD) Design-Expertreg version 11 software
24 Quantitative Phytochemical Analysis +e leaf extractthat exhibited the maximum antibacterial activity wasassessed for the presence of phytochemicals A preliminaryphytochemical analysis was performed to determine theamount of phenolic and flavonoid compounds in milligramper gram of extracted powder [36ndash38]
25 Determination of Total Phenolic Content (TPC)UV-spectrophotometric methods are most commonly usedfor the quantification of phenolic content Preparation ofstandard gallic acid solution was as follows 02 gram of gallicacid was dissolved into 200ml distilled water so the con-centration of the solution was 0001 gramml or 1000 microgml+is is called the stock solution +en serial dilution wasperformed in order to prepare different concentrations ofthe solution (0 gml 50 gml 100mgml 150mgml200mgml 250mgml and 300mgml) which are used forpreparing calibration curve
Estimation of total phenol content in the selected plantextract was measured spectrophotometrically byFolinndashCiocalteu (FCR) colorimetric method using gallicacid as the standard and expressing results as gallic acidequivalent (GAE) per gram of sample Different concen-trations (001mgml) of gallic acid were prepared inmethanol Aliquots of 1ml of the test sample and eachsample of the standard solution were taken and mixed with2ml of FolinndashCiocalteu reagent (1 10 in deionized water)and 4ml of a saturated solution of sodium carbonate (75wv) +e tubes were covered with silver foils and incubatedat room temperature for 30 minutes with intermittentshaking +e absorbance was taken at 765 nm using meth-anol as blank All the samples were analyzed in three rep-lications +e total phenolic amount was determined withthe help of a standard cure prepared from a pure phenolicstandard (gallic acid) [10 39 40]
TPCmgGAE
m1113874 1113875
ClowastV
m (1)
A formula was used to assess the phenolic compoundsin mg from one gram of extracted powder when the TPCamount increases the antibacterial activity will be effective
Here TPC is the total phenol content in mg of gallic acidequivalent per gram of extracted gallic acid equivalent m isdry mass of a sample in gram used for characterization C is aconcentration of gallic acid in mgl and V is the volume ofsample taken in a milliliter
26 Determination of Total Flavonoid Content (TFC) +eTFC of the leaf extract was determined by aluminumchloride colorimetric assay Briefly 05ml aliquots of theextract and standard solution (001ndash10mgml) of quercetinwere added to 2ml of distilled water and subsequently to015ml of sodium nitrite (5 NaNO2 wv) solution andmixed After 6 minutes 015ml of (10 AlCl3 wv) solutionwas added+e solutions were allowed to stand for quercetin6min and after that 2ml of sodium hydroxide (4 NaOHwv) solution was added to the mixture +e final volumewas adjusted to 5ml with immediate addition of distilled
Journal of Chemistry 3
water mixed thoroughly and allowed to stand for another15min +e absorbance of each mixture was determined at510 nm against the samemixture but without leaf extract as ablank TFC was determined as mg quercetin equivalent pergram of sample with the help of the calibration curve ofquercetin All measurements were performed in triplicate(n 3) [41]
TFCmgQUE
m1113874 1113875
ClowastV
m (2)
+e total flavonoid content of the extracts can be de-termined using the above formula where C is the concen-tration of quercetin in mgL of quercetin equivalence V isthe volume of sample taken (ml) m is the dry weight of
sample (g) and TFC is the total flavonoid content in mg ofquercetin equivalence
27 Functional Group and 4ermal Analysis FourierTransform Infrared (FTIR) Spectrophotometer is the mostpowerful tool for identifying the types of functional groupsbased on the wavelength of light absorbed By interpretingthe infrared absorption spectrum the chemical bonds in amolecule were determined [42]
+e TGA curve was obtained with a heating rate of10degCminminus1 in the temperature range of 30 to 1000degC byusing alumina crucibles and samplesrsquo mass of about 10mg+e experiments were carried out under the nitrogen at-mosphere at a flow rate of 50mlminminus1
28 Application Procedure Pad-Dry-Cure is most widelyused for 100 scoured cotton fabric Nettle leaf extractedpowder was treated with nine percent on weight of fabric(owf) under room temperature +e treated fabric waspassed between the rollers two to three times at a uniformpressure at 15 bar for better penetration of finishing agentand to squeeze out excess liquid from the fabric +e fabricwas then dried at 110degC and cured at 130degC in a curingchamber within 3 minutes
29 Antibacterial Test Antibacterial testing was done byAATCC standard test method 1002004 for the quantitativevaluation of the antibacterial effectiveness of the antimi-crobial agents against Gram-positive bacteria (Staphylo-coccus aureus) and Gram-negative bacteria (Escherichiacoli) Assessment of the percent reduction of bacteria wascalculated using
R() B minus A
B1113874 1113875 times 100 (3)
R is the percent reduction of bacteria A is the thenumber of bacteria recovered from the inoculated treatedtest specimen swatches in the jar incubated over the desiredcontact period B is the the number of bacteria recoveredfrom the inoculated untreated test specimen swatches in thejar incubated over the desired contact period microbes anddyed fabric
HO
HO
OH
OH
O
O
O
O
(a)
HO
HOHO
HO
OH
OH
OH
OH
H3C
OH
OH
O
OO
O
O
O
(b)
Figure 1 Chemical structures of extracted phenolic compound (a) 2-O-caffeoylmalic acid (b) rutin [33 34]
Table 1 Antibacterial agent extraction parameters water andethanol used as extraction solvents
Extraction factors ParametersMaterial to liquor ratio 1 10 1 20 1 30Extraction time (minutes) 30 60 90Extraction temperature (degC) 45ndash50
Table 2 Number of runs by using central composite design (CCD)and their yield
210 Wash Durability Test +e treated fabrics were laun-dered using AATCC test method 61 Laundering was carriedout at MLR of 1 10 with 05 on weight of fabric of AATCCdetergent and 100 steel balls at a temperature of 90degC for 30minutes +e washing cycle was followed by hot rinsing inplain water at 40degC for 10 minutes Finally the washedswatches were tumble-dried Since a single wash-dry cyclesimulated 8 regular wash cycles the laundering procedurewas repeated 5 10 15 20 25 30 35 and 40 times to checkchemical durability
3 Results and Discussion
31 Yield of Extraction Using Water and Ethanol +e ex-perimental results (Table 2) can be illustrated by the fol-lowing linear equation
Yield 1015076 + 033 time + 0497487 conc (4)
Yield 1498065 + 031 Time + 0497487Conc (5)
Equations (4) and (5) depict the yield that has a linearrelationship with the factor of extraction time and con-centration of water and ethanol used as extraction solventrespectively
+e actual value and model prediction value of the yieldshowed a good correlation (Figure 2) Based on the ANOVAanalysis the linear equation has a p-value of 00001 (lt005)indicating that the equation model is significant
32 Analysis of Variance (ANOVA) +e results of theANOVA analysis factors A and B had a significant effect(Tables 3 and 4) +e factors A and B had a p-value of 00001and 00001 respectively +e model showed that the factorsA and B had a positive effect on the extraction yield indi-cating an increase in these factors extraction yield increases(Figure 3)
33 Optimization Extraction Parameters +e optimumconditions are based on the resulting desirability value +egoal of extraction is to minimize extraction time concen-tration and maximum water and ethanol extraction yield asshown in Tables 5 and 6 respectively +e optimizationprocess was performed by establishing the highest level ofextraction yield
Table 7 shows that the optimal extraction time is 59minutes with concentration of 10mlg the predictiveyield is 34991 percent Ethanolic extraction yield hasoptimal extraction time of 59026 minute with concen-tration of 10458mlg the predictive yield is 38716percent (Table 8)
34 Quantitative Analysis of Phytochemical Ingredients+e amount of total phenol content in the extract was de-termined by the Folin-Ciocalteau reagent described in theMaterials and Methods section using gallic acid as thestandard +e absorbance values obtained at differentconcentrations of gallic acid were used for the construction
of a calibration curve It appeared that the extraction ofnettle plant leaf total phenolic content is 27819plusmn 0131mgGAEg dry weight (equation (1))+e total flavonoid contentin the extract of nettle plant leaves is 2566plusmn 0227mgGAEgdry weight (equation (2)) [43ndash46]
FTIR studied in extracted nettle leaf displayed strongabsorption peaks at 307819 cmminus1 154929 cmminus1 140509 cmminus1and 107781 cmminus1 +e broad peak between 3500 cmminus1 and2500 cmminus1 corresponds to a strong O-H stretch vibrationwhich indicates the presence of hydroxyl groups in nettle leafextract On finger print region a doublet band is presentbetween1390 cmminus1 and 1310 cmminus1 representing O-H bendingwhich indicates phenolic compounds +e FTIR spectra of thetreated and untreated cotton fabric were almost the same andslight differences were at wave number 3000ndash2500 cmminus1 +etreated fabric has O-H stretch vibration and OH functionalgroup between 3000 and 2500 cmminus1 (Figure 4(a))
+e TGA curves of the crude extract showed that asmall weight loss was found in the range of 90ndash162degC dueto the evaporation of the humidity of the materials orvolatile compounds 162ndash537degC was associated with ali-phatic phenolic compounds decomposition or degrada-tion Char formation was detected between 537 and1028degC by further extending the analysis temperature(Figure 4(b))
35 Effect of Tensile Strength +e tensile strength of the Pad-Dry-Cure treated cotton fabric decreased by 066 and 117percent compared to the untreated control in warp and weftdirection respectively
Other physical properties such as permeability stiffnessstrength and absorbency were tested accordingly based onASTM ISO and AATCC standard respectively [33 47]
36 ReactionMechanisms +e two carboxylic groups of thecitric acid are linked with the hydroxyl part of the celluloseand with extracted phenol through covalent bond (Figure 5)+eir effective antibacterial activity and phenolic com-pounds were attached to cotton fabric using citric acid as acrosslinker Phenolic compounds are among the major anddiverse groups of active compounds in the nettle plant leafCotton fabrics treated with phenolic compounds showedexcellent antibacterial activity against the Gram-positivebacteria Staphylococcus aureus as well as the Gram-negativebacteria Escherichia coli
37AntibacterialActivity +e Pad-Dry-Cure treated fabricexhibited maximum antibacterial activity against Gram-negative test organisms compared to the Gram-positivetest organisms Maximum bacteria reduction was observedagainst Staphylococcus aureus and Escherichia coli whenthe padding mangle was applied at a pressure of 15 barwith 20 30 and 40 minutes of wetting time +is resultdemonstrated that the higher the wetting time (30 minutesand 40 minutes) in padding the better the antibacterialproperties At lower wetting time 20 minutes the anti-bacterial property is low as compared to the other wetting
Journal of Chemistry 5
Predicted vs actual
Color points by value ofyield25 55
30 35 40 504525 55Actual
25
30
35
40
45
50
55Pr
edic
ted
(a)
Color points by value ofyield29 59
Predicted vs actual
30 40 5020 60Actual
20
30
40
50
60
Pred
icte
d
(b)
Figure 2 Correlation between actual value and predicted value of (a) water and (b) ethanol extraction yield
Table 3 Analysis of variance (ANOVA) of the water extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 98997 2 49499 244408 lt00001
SignificantA time 79198 1 79198 391052 lt00001B conc 19799 1 19799 97763 lt00001Residual 203 10 02025Lack of fit 00253 6 00042 00084 10000 Not significantPure error 200 4 05000Cor total 99200 12
Table 4 Analysis of variance (ANOVA) of the ethanol extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 90780 2 45390 53341 lt00001
SignificantA time 70980 1 70980 83415 lt00001B conc 19799 1 19799 23268 lt00001Residual 851 10 08509Lack of fit 651 6 108 217 02367 Not significantPure error 200 4 05000Cor total 91631 12
Yield ()
Yiel
d (
)
55
50
45
40
35
30
25
25
20B concentration (mlg)
A time (m
inute)
1510 30
4050
6070
809030
Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
25 55
(a)
Yiel
d (
)
60
50
40
30
20
B concentration (mlg) A time (m
inute)25
2015
10 3040
5060
7080
9030
Yield ()Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
29 59
(b)
Figure 3 Interaction of factors time and temperature on (a) water and (b) ethanol extraction yield
Table 7 Optimization at minimum time concentration and high yield
Number Time (min) Conc(mlg) Yield () Desirability1 59896 10000 34991 0551 Selected
Table 8 Optimization at minimum time concentration and high yield
Number Time (min) Concentration (mlg) Yield Desirability1 59026 10458 38716 0547 Selected
008
006
004
002
000
4000 3500 3000 2500 2000Wave number (cmndash1)
1500 1000 500 0
Abso
rban
ce (
)
Untreated fabricTreated fabric dry
Powder extractedPowder
(a)
1000800600Temperature (degC)4002000
0
ndash5
ndash10
ndash15
ndash20
Mas
s los
s (m
g)
ndash25
ndash30
1200
(b)
Figure 4 Functional group and thermal analysis of nettle leaf extracted powder (a) combined FTIR spectra of untreated cotton fabric (b)thermography resulting from TGA analysis obtained under a nitrogen flow of 50mlmin and heating rate of 10degCmin
+
+
H
H C COOHH
H C C
O
O
OOC
HO C COOH
H
H
CHO
OH ndash celluloseCellulose
OH
RR R
R
RR
R
R
RR
C COOH
H
H
CCOOH
Citric acid Phenol derivatives
Figure 5 Mechanism of reaction between cellulose citric acid and phenolic compounds [48]
Journal of Chemistry 7
time +is effect could be becuase the longer the wettingtime of each particle of the extracted agents the deeper thepenetration inside the cotton fiber and the better thedurability (Table 9 Figure 6)
38 Durability to Laundering Generally the finishedscoured cotton fabric subjected to number of wash cycles (510 15 20 25 30 35 and 40) showed a gradual decrease inantibacterial property with 100 to 44 reduction in thebacterial count for Staphylococcus aureus and 100 to 30reduction in the bacterial count for Escherichia coli(Figure 7)
Citric acid as a crosslinking agent was added to theantibacterial finishing solutions It was found that the citric
acid was fairly effective against bacteria Adding poly-carboxylic acids to the antibacterial finishing recipes willenhance the durability of many laundering cycles
4 Conclusion
Natural and eco-friendly antibacterial finishing of textiles astrong antibacterial finishing of textile substrates withgood fastness and stability was obtained with nettle leafextract crosslinking on cotton fabrics using citric acid Itexhibits higher antibacterial efficiency +ere was a 100 to9975 percent reduction in the count of test bacteria afterPad-Dry-Cure treatment of the scoured cotton fabrics withthe dry nettle leaf extracted with optimized variables +eoptimization of the Pad-Dry-Cure conditions for finishing
S aureusSoaking time-20 minutes
S aureusSoaking time-30 minutes
S aureusSoaking time-40 minutes
E coliSoaking time-20 minutes
E coliSoaking time-30 minutes
E coliSoaking time-40 minutes
Figure 6 +e test results of Pad-Dry-Cure antibacterial treated fabric for Staphylococcus aureus and Escherichia coli
Aer 5 wash Aer 10 wash Aer 15 wash Aer 20 wash
Aer 25 wash Aer 30 wash Aer 35 wash Aer 40 wash
Figure 7 +e test results of wash durability for the treated fabrics (note A Escherichia coli B Staphylococcus aureus)
Table 9 Bacterial reduction test on the Pad-Dry-Cure treated fabric
was assessed for bacterial reduction test against Escherichiacoli and Staphylococcus aureus Maximum bacterial re-duction percentage was observed against Staphylococcusaureus and Escherichia coli when the wetting time was 30and 40minutes
Data Availability
+e authors have annotated the entire data building processthe empirical techniques presented in the paper and thenumber of runs generated using Design-Expert and Minitab18 software for optimization and analyzation based on theirparameters All data used to support the findings of thisstudy are included within the paper
Conflicts of Interest
Asnake Ketema is currently working as a lecturer in textilechemistry at Dire Dawa Institute of Technology Dire DawaUniversity Dire Dawa Ethiopia Amare Worku is cur-rently working as lecturer in textile chemistry and SchoolDean of the School of Textile Apparel and Fashion Designat Dire Dawa Institute of Technology Dire Dawa Uni-versity Dire Dawa Ethiopia +e authors declare that thereare no conflicts of interest regarding the publication of thispaper
Acknowledgments
+e authors would like to thank their advisor Dr GNalankilli professor of textile chemistry for his supportinvaluable guidance and constructive criticism during thesiswork and Dr Tamrat Tesfaye the secretary of the committeefor his encouragement and hard questions +is work wouldnot have been possible without the financial support of theEthiopian Institute of Textile and Fashion Technology(EiTEX) only for research work
References
[1] A Kalia B Joshi and M Mukhija ldquoPharmacognostical re-view of Urtica dioica Lrdquo International Journal of GreenPharmacy (IJGP) vol 8 no 4 pp 1998ndash4103 2014
[2] J Sheikh N Singh and M Srivastava ldquoFunctional dyeing ofcellulose-based (linen) fabric using Bombax ceiba (kapok)flower extractrdquo Fibers and Polymers vol 20 no 2 pp 312ndash319 2019
[3] L Qian ldquoApplication of nanotechnology for high perfor-mance textilesrdquo Journal of Textile and Apparel Technologyand Management vol 4 no 1 pp 1ndash7 2004
[4] C K Kang S S Kim S Kim et al ldquoAntibacterial cotton fiberstreated with silver nanoparticles and quaternary ammoniumsaltsrdquo Carbohydrate Polymers vol 151 pp 1012ndash1018 2016
[5] J E Herrera ldquoSynthesis of nanodispersed oxides of vanadiumtitanium molybdenum and tungsten on Mesoporous silicausing atomic layer depositionrdquo Topics in Catalysis vol 39no 3-4 pp 245ndash255 2006
[6] J Hudec M Burdova L u Kobida et al ldquoAntioxidant ca-pacity changes and phenolic profile of Echinacea purpureanettle (Urtica dioica L) and dandelion (Taraxacum officinale)after application of polyamine and phenolic biosynthesis
regulatorsrdquo Journal of Agricultural and Food Chemistryvol 55 no 14 pp 5689ndash5696 2007
[7] N A Ibrahim M H Abo-Shosha M A GaffarA M Elshafei and O M Abdel-Fatah ldquoAntibacterialproperties of ester-cross-linked cellulose-containing fabricspost-treated with metal saltsrdquo Polymer-Plastics Technologyand Engineering vol 45 no 6 pp 719ndash727 2006
[8] G +ilagavathi and S K Bala ldquoMicroencapsulation of herbalextracts for microbial resistance in healthcare textilesrdquoJournal of Fiber and Textile Research vol 32 no 1 pp 351ndash354 2007
[9] N A Salih ldquoAntibacterial effect of nettle (Urtica dioica)rdquo Al-Qadisiyah Journal of Veterinary Medicine Sciences vol 13no 1 p 1 2014
[10] K K Ghaima N M Hashim and S A Ali ldquoAntibacterial andantioxidant activities of ethyl acetate extract of nettle (Urticadioica) and dandelion (Taraxacum officinale)rdquo Journal ofApplied Pharmaceutical Science vol 3 no 5 p 96 2013
[11] T L Vigo Protection of Textiles from Biological AttackWoodhead Publishing Sawston UK 1st edition 2005
[12] S Hashemikia andMMontazer ldquoSodium hypophosphite andnano TiO2 inorganic catalysts along with citric acid on textileproducing multi-functional propertiesrdquo Applied Catalysis AGeneral vol 417-418 pp 200ndash208 2012
[13] M Montazer and M G Afjeh ldquoSimultaneous x-linking andantimicrobial finishing of cotton fabricrdquo Journal of AppliedPolymer Science vol 103 no 1 pp 178ndash185 2007
[14] R Aladpoosh and M Montazer ldquo+e role of cellulosic chainsof cotton in biosynthesis of ZnO nanorods producing mul-tifunctional properties mechanism characterizations andfeaturesrdquo Carbohydrate Polymers vol 126 pp 122ndash129 2015
[15] PS Vankar ldquoAntibacterial and antioxidant activities of ethylacetate extract of nettle (Urtica dioica) and dandelion (Tar-axacum officinale)rdquo Journal of Applied Pharmaceutical Sci-ence vol 3 pp 096ndash099 2013
[16] T Nithya J Jayanthi and M Ragunathan ldquoAntioxidantactivity total phenol flavonoid alkaloid tannin and saponincontents of leaf extracts of Salvinia molesta DS MitchellrdquoAsian Journal of Pharmaceutical and Clinical Research vol 9no 1 pp 200ndash203 2016
[17] R Roghini and K J Vijayalakshmi ldquoPhytochemical screen-ing quantitative analysis of flavonoids and minerals inethanolic extract of citrus paradisirdquo International Journal ofPharmaceutical Sciences and Research vol 9 no 11pp 4859ndash4864 2018
[18] F Sidaoui ldquoStudy of Tunisian nettle leaves (Urtica dioica L)mineral composition and antioxidant capacity of their ex-tracts obtained by maceration and supercritical fluid ex-tractionrdquo International Journal of Pharmacognosy andPhytochemical Research vol 7 pp 707ndash713 2015
[19] B Simoncic and B Tomsic ldquoStructures of novel antimicrobialagents for textiles-a reviewrdquo Textile Research Journal vol 80no 16 pp 1721ndash1737 2010
[20] G Sun and S D Worley ldquoChemistry of durable and re-generable biocidal textilesrdquo Journal of Chemical Educationvol 82 no 1 p 60 2005
[21] P Jaswal S AgyaPreet and G J Goel ldquoAntimicrobial activityof herbal treated cotton fabricrdquo International ResearchJournal of Engineering and Technology vol 4 no 8 pp 39ndash432017
[22] M Sathianarayanan ldquoAntibacterial finish for cotton fabricfrom herbal productsrdquo Indian Journal of Fiber and TextileResearch vol 35 pp 50ndash58 2010
Journal of Chemistry 9
[23] D Kut ldquoEffects of environmental conditions on the anti-bacterial activity of treated cotton knitsrdquo AATCC Reviewvol 5 no 3 2005
[24] N Afraz ldquoAntimicrobial finishes for textilesrdquo Including re-sults for Curr Trends Fashion Technology Textile Engineeringvol 5 p 4 2019
[25] A El-Shafei ldquoHerbal extract as an ecofriendly antibacterialfinishing of cotton fabricrdquo Egyptian Journal of Chemistryvol 61 no 2 pp 317ndash327 2018
[26] A Haji M Nasiriboroumand and S S Qavamnia ldquoCottondyeing and antibacterial finishing using agricultural waste byan eco-friendly process optimized by response surfacemethodologyrdquo Fibers and Polymers vol 19 no 11pp 2359ndash2364 2018
[27] A Reshma V B Priyadarisini and K Amutha ldquoSustainableantimicrobial finishing of fabrics using natural bioactiveagentsrdquo International Journal of Life Science vol 4 pp 10ndash202018
[28] W Ibrahim ldquoAloe vera leaf gel extract for antibacterial andsoftness properties of cottonrdquo Journal of Textile Science ampEngineering vol 7 no 301 p 2 2017
[29] P S Vankar R Shanker and S Wijayapala ldquoDyeing ofcotton wool and silk with extract of Allium cepardquo Pigment ampResin Technology vol 38 no 4 pp 242ndash247 2009
[30] G Singh ldquoFunctionalization of wool fabric using kapokflower and bio-mordantrdquo Sustainable Chemistry and Phar-macy vol 14 pp 2352ndash5541 2019
[31] K Gong Y Pan L J Rather et al ldquoNatural pigment duringflora leaf senescence and its application in dyeing and UVprotection finish of silk and woolmdasha case study of Cinna-momum camphorardquoDyes and Pigments vol 166 pp 114ndash1212019
[32] J Sheikh ldquoUltrasound assisted extraction of natural dyes andnatural mordants vis a vis dyeingrdquo Fibers and Polymersvol 17 no 5 pp 738ndash743 2016
[33] K Koszegi ldquoAntimicrobial Effects of the stinging nettle(Urtica dioica L)rdquo Analecta Technical Szegedinensia vol 11p 22 2017
[34] K Belay andM J C M R Sisay ldquoPhytochemical constituentsand physicochemical properties of medicinal plant (Moringaoleifera) around Bule Horardquo Chemistry and Materials Re-search vol 6 no 7 pp 61ndash72 2014
[35] K Murugesh Babu and K B Ravindra ldquoBioactive antimi-crobial agents for finishing of textiles for health care prod-uctsrdquo 4e Journal of the Textile Institute vol 106 no 7pp 706ndash717 2015
[36] I Gulccedilin ldquoAntioxidant antimicrobial antiulcer and analgesicactivities of nettle (Urtica dioica L)rdquo Journal of Ethno-pharmacology vol 90 no 2-3 pp 205ndash215 2004
[37] P Mantecca E Moschini P Bonfanti et al ldquoToxicity eval-uation of a new Zn-doped CuO nanocomposite with highlyeffective antibacterial propertiesrdquo Toxicological Sciencesvol 146 no 1 pp 16ndash30 2015
[38] V K Midha A Dakuri and V Midha ldquoStudies on theproperties of nonwoven surgical gownsrdquo Journal of IndustrialTextiles vol 43 no 2 pp 174ndash190 2013
[39] S W Ali S Rajendran and M Joshi ldquoSynthesis and char-acterization of chitosan and silver loaded chitosan nano-particles for bioactive polyesterrdquo Carbohydrate Polymersvol 83 no 2 pp 438ndash446 2011
[40] G M L Bearman A Rosato K Elam et al ldquoA crossover trialof antimicrobial scrubs to reduce methicillin-resistantStaphylococcus aureus burden on healthcare worker apparelrdquo
Infection Control amp Hospital Epidemiology vol 33 no 3pp 268ndash275 2012
[41] F Eser and A Onal ldquoDyeing of wool and cotton with extractof the nettle (Urtica dioica L) leavesrdquo Journal of NaturalFibers vol 12 no 3 pp 222ndash231 2015
[42] G Bag ldquoAssessment of total flavonoid content and antioxi-dant activity of methanolic rhizome extract of threeHedychium species of Manipur valleyrdquo International Journalof Pharmaceutical Sciences vol 30 no 1 pp 154ndash159 2015
[43] S ETHurovic ldquoChemical composition of stinging nettle leavesobtained by different analytical approachesrdquo Journal ofFunctional Food vol 32 pp 18ndash26 2017
[44] C S Ezeonu and C M Ejikeme ldquoQualitative and quantitativedetermination of phytochemical contents of indigenousNigerian softwoodsrdquo New Journal of Science vol 56 ArticleID 5601327 9 pages 2016
[45] H Y Fu S J Chen R F Chen W H Ding L L Kuo-Huangand R N Huang ldquoIdentification of oxalic acid and tartaricacid as major persistent pain-inducing toxins in the stinginghairs of the nettle Urtica thunbergianardquo Annals of Botanyvol 98 no 1 pp 57ndash65 2006
[46] Y Gao and R Cranston ldquoRecent advances in antimicrobialtreatments of textilesrdquo Textile Research Journal vol 78 no 1pp 60ndash72 2008
[47] S W Ali ldquoAntibacterial properties of aloe vera gel-finishedcotton fabricrdquo Cellulose vol 21 no 3 pp 2063ndash2072 2014
[48] M Gupta S +akur A Sharma and S Gupta ldquoQualitativeand quantitative analysis of phytochemicals and pharmaco-logical value of some dye yielding medicinal plantsrdquo OrientalJournal of Chemistry vol 29 no 2 pp 475ndash481 2013
10 Journal of Chemistry
water mixed thoroughly and allowed to stand for another15min +e absorbance of each mixture was determined at510 nm against the samemixture but without leaf extract as ablank TFC was determined as mg quercetin equivalent pergram of sample with the help of the calibration curve ofquercetin All measurements were performed in triplicate(n 3) [41]
TFCmgQUE
m1113874 1113875
ClowastV
m (2)
+e total flavonoid content of the extracts can be de-termined using the above formula where C is the concen-tration of quercetin in mgL of quercetin equivalence V isthe volume of sample taken (ml) m is the dry weight of
sample (g) and TFC is the total flavonoid content in mg ofquercetin equivalence
27 Functional Group and 4ermal Analysis FourierTransform Infrared (FTIR) Spectrophotometer is the mostpowerful tool for identifying the types of functional groupsbased on the wavelength of light absorbed By interpretingthe infrared absorption spectrum the chemical bonds in amolecule were determined [42]
+e TGA curve was obtained with a heating rate of10degCminminus1 in the temperature range of 30 to 1000degC byusing alumina crucibles and samplesrsquo mass of about 10mg+e experiments were carried out under the nitrogen at-mosphere at a flow rate of 50mlminminus1
28 Application Procedure Pad-Dry-Cure is most widelyused for 100 scoured cotton fabric Nettle leaf extractedpowder was treated with nine percent on weight of fabric(owf) under room temperature +e treated fabric waspassed between the rollers two to three times at a uniformpressure at 15 bar for better penetration of finishing agentand to squeeze out excess liquid from the fabric +e fabricwas then dried at 110degC and cured at 130degC in a curingchamber within 3 minutes
29 Antibacterial Test Antibacterial testing was done byAATCC standard test method 1002004 for the quantitativevaluation of the antibacterial effectiveness of the antimi-crobial agents against Gram-positive bacteria (Staphylo-coccus aureus) and Gram-negative bacteria (Escherichiacoli) Assessment of the percent reduction of bacteria wascalculated using
R() B minus A
B1113874 1113875 times 100 (3)
R is the percent reduction of bacteria A is the thenumber of bacteria recovered from the inoculated treatedtest specimen swatches in the jar incubated over the desiredcontact period B is the the number of bacteria recoveredfrom the inoculated untreated test specimen swatches in thejar incubated over the desired contact period microbes anddyed fabric
HO
HO
OH
OH
O
O
O
O
(a)
HO
HOHO
HO
OH
OH
OH
OH
H3C
OH
OH
O
OO
O
O
O
(b)
Figure 1 Chemical structures of extracted phenolic compound (a) 2-O-caffeoylmalic acid (b) rutin [33 34]
Table 1 Antibacterial agent extraction parameters water andethanol used as extraction solvents
Extraction factors ParametersMaterial to liquor ratio 1 10 1 20 1 30Extraction time (minutes) 30 60 90Extraction temperature (degC) 45ndash50
Table 2 Number of runs by using central composite design (CCD)and their yield
210 Wash Durability Test +e treated fabrics were laun-dered using AATCC test method 61 Laundering was carriedout at MLR of 1 10 with 05 on weight of fabric of AATCCdetergent and 100 steel balls at a temperature of 90degC for 30minutes +e washing cycle was followed by hot rinsing inplain water at 40degC for 10 minutes Finally the washedswatches were tumble-dried Since a single wash-dry cyclesimulated 8 regular wash cycles the laundering procedurewas repeated 5 10 15 20 25 30 35 and 40 times to checkchemical durability
3 Results and Discussion
31 Yield of Extraction Using Water and Ethanol +e ex-perimental results (Table 2) can be illustrated by the fol-lowing linear equation
Yield 1015076 + 033 time + 0497487 conc (4)
Yield 1498065 + 031 Time + 0497487Conc (5)
Equations (4) and (5) depict the yield that has a linearrelationship with the factor of extraction time and con-centration of water and ethanol used as extraction solventrespectively
+e actual value and model prediction value of the yieldshowed a good correlation (Figure 2) Based on the ANOVAanalysis the linear equation has a p-value of 00001 (lt005)indicating that the equation model is significant
32 Analysis of Variance (ANOVA) +e results of theANOVA analysis factors A and B had a significant effect(Tables 3 and 4) +e factors A and B had a p-value of 00001and 00001 respectively +e model showed that the factorsA and B had a positive effect on the extraction yield indi-cating an increase in these factors extraction yield increases(Figure 3)
33 Optimization Extraction Parameters +e optimumconditions are based on the resulting desirability value +egoal of extraction is to minimize extraction time concen-tration and maximum water and ethanol extraction yield asshown in Tables 5 and 6 respectively +e optimizationprocess was performed by establishing the highest level ofextraction yield
Table 7 shows that the optimal extraction time is 59minutes with concentration of 10mlg the predictiveyield is 34991 percent Ethanolic extraction yield hasoptimal extraction time of 59026 minute with concen-tration of 10458mlg the predictive yield is 38716percent (Table 8)
34 Quantitative Analysis of Phytochemical Ingredients+e amount of total phenol content in the extract was de-termined by the Folin-Ciocalteau reagent described in theMaterials and Methods section using gallic acid as thestandard +e absorbance values obtained at differentconcentrations of gallic acid were used for the construction
of a calibration curve It appeared that the extraction ofnettle plant leaf total phenolic content is 27819plusmn 0131mgGAEg dry weight (equation (1))+e total flavonoid contentin the extract of nettle plant leaves is 2566plusmn 0227mgGAEgdry weight (equation (2)) [43ndash46]
FTIR studied in extracted nettle leaf displayed strongabsorption peaks at 307819 cmminus1 154929 cmminus1 140509 cmminus1and 107781 cmminus1 +e broad peak between 3500 cmminus1 and2500 cmminus1 corresponds to a strong O-H stretch vibrationwhich indicates the presence of hydroxyl groups in nettle leafextract On finger print region a doublet band is presentbetween1390 cmminus1 and 1310 cmminus1 representing O-H bendingwhich indicates phenolic compounds +e FTIR spectra of thetreated and untreated cotton fabric were almost the same andslight differences were at wave number 3000ndash2500 cmminus1 +etreated fabric has O-H stretch vibration and OH functionalgroup between 3000 and 2500 cmminus1 (Figure 4(a))
+e TGA curves of the crude extract showed that asmall weight loss was found in the range of 90ndash162degC dueto the evaporation of the humidity of the materials orvolatile compounds 162ndash537degC was associated with ali-phatic phenolic compounds decomposition or degrada-tion Char formation was detected between 537 and1028degC by further extending the analysis temperature(Figure 4(b))
35 Effect of Tensile Strength +e tensile strength of the Pad-Dry-Cure treated cotton fabric decreased by 066 and 117percent compared to the untreated control in warp and weftdirection respectively
Other physical properties such as permeability stiffnessstrength and absorbency were tested accordingly based onASTM ISO and AATCC standard respectively [33 47]
36 ReactionMechanisms +e two carboxylic groups of thecitric acid are linked with the hydroxyl part of the celluloseand with extracted phenol through covalent bond (Figure 5)+eir effective antibacterial activity and phenolic com-pounds were attached to cotton fabric using citric acid as acrosslinker Phenolic compounds are among the major anddiverse groups of active compounds in the nettle plant leafCotton fabrics treated with phenolic compounds showedexcellent antibacterial activity against the Gram-positivebacteria Staphylococcus aureus as well as the Gram-negativebacteria Escherichia coli
37AntibacterialActivity +e Pad-Dry-Cure treated fabricexhibited maximum antibacterial activity against Gram-negative test organisms compared to the Gram-positivetest organisms Maximum bacteria reduction was observedagainst Staphylococcus aureus and Escherichia coli whenthe padding mangle was applied at a pressure of 15 barwith 20 30 and 40 minutes of wetting time +is resultdemonstrated that the higher the wetting time (30 minutesand 40 minutes) in padding the better the antibacterialproperties At lower wetting time 20 minutes the anti-bacterial property is low as compared to the other wetting
Journal of Chemistry 5
Predicted vs actual
Color points by value ofyield25 55
30 35 40 504525 55Actual
25
30
35
40
45
50
55Pr
edic
ted
(a)
Color points by value ofyield29 59
Predicted vs actual
30 40 5020 60Actual
20
30
40
50
60
Pred
icte
d
(b)
Figure 2 Correlation between actual value and predicted value of (a) water and (b) ethanol extraction yield
Table 3 Analysis of variance (ANOVA) of the water extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 98997 2 49499 244408 lt00001
SignificantA time 79198 1 79198 391052 lt00001B conc 19799 1 19799 97763 lt00001Residual 203 10 02025Lack of fit 00253 6 00042 00084 10000 Not significantPure error 200 4 05000Cor total 99200 12
Table 4 Analysis of variance (ANOVA) of the ethanol extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 90780 2 45390 53341 lt00001
SignificantA time 70980 1 70980 83415 lt00001B conc 19799 1 19799 23268 lt00001Residual 851 10 08509Lack of fit 651 6 108 217 02367 Not significantPure error 200 4 05000Cor total 91631 12
Yield ()
Yiel
d (
)
55
50
45
40
35
30
25
25
20B concentration (mlg)
A time (m
inute)
1510 30
4050
6070
809030
Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
25 55
(a)
Yiel
d (
)
60
50
40
30
20
B concentration (mlg) A time (m
inute)25
2015
10 3040
5060
7080
9030
Yield ()Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
29 59
(b)
Figure 3 Interaction of factors time and temperature on (a) water and (b) ethanol extraction yield
Table 7 Optimization at minimum time concentration and high yield
Number Time (min) Conc(mlg) Yield () Desirability1 59896 10000 34991 0551 Selected
Table 8 Optimization at minimum time concentration and high yield
Number Time (min) Concentration (mlg) Yield Desirability1 59026 10458 38716 0547 Selected
008
006
004
002
000
4000 3500 3000 2500 2000Wave number (cmndash1)
1500 1000 500 0
Abso
rban
ce (
)
Untreated fabricTreated fabric dry
Powder extractedPowder
(a)
1000800600Temperature (degC)4002000
0
ndash5
ndash10
ndash15
ndash20
Mas
s los
s (m
g)
ndash25
ndash30
1200
(b)
Figure 4 Functional group and thermal analysis of nettle leaf extracted powder (a) combined FTIR spectra of untreated cotton fabric (b)thermography resulting from TGA analysis obtained under a nitrogen flow of 50mlmin and heating rate of 10degCmin
+
+
H
H C COOHH
H C C
O
O
OOC
HO C COOH
H
H
CHO
OH ndash celluloseCellulose
OH
RR R
R
RR
R
R
RR
C COOH
H
H
CCOOH
Citric acid Phenol derivatives
Figure 5 Mechanism of reaction between cellulose citric acid and phenolic compounds [48]
Journal of Chemistry 7
time +is effect could be becuase the longer the wettingtime of each particle of the extracted agents the deeper thepenetration inside the cotton fiber and the better thedurability (Table 9 Figure 6)
38 Durability to Laundering Generally the finishedscoured cotton fabric subjected to number of wash cycles (510 15 20 25 30 35 and 40) showed a gradual decrease inantibacterial property with 100 to 44 reduction in thebacterial count for Staphylococcus aureus and 100 to 30reduction in the bacterial count for Escherichia coli(Figure 7)
Citric acid as a crosslinking agent was added to theantibacterial finishing solutions It was found that the citric
acid was fairly effective against bacteria Adding poly-carboxylic acids to the antibacterial finishing recipes willenhance the durability of many laundering cycles
4 Conclusion
Natural and eco-friendly antibacterial finishing of textiles astrong antibacterial finishing of textile substrates withgood fastness and stability was obtained with nettle leafextract crosslinking on cotton fabrics using citric acid Itexhibits higher antibacterial efficiency +ere was a 100 to9975 percent reduction in the count of test bacteria afterPad-Dry-Cure treatment of the scoured cotton fabrics withthe dry nettle leaf extracted with optimized variables +eoptimization of the Pad-Dry-Cure conditions for finishing
S aureusSoaking time-20 minutes
S aureusSoaking time-30 minutes
S aureusSoaking time-40 minutes
E coliSoaking time-20 minutes
E coliSoaking time-30 minutes
E coliSoaking time-40 minutes
Figure 6 +e test results of Pad-Dry-Cure antibacterial treated fabric for Staphylococcus aureus and Escherichia coli
Aer 5 wash Aer 10 wash Aer 15 wash Aer 20 wash
Aer 25 wash Aer 30 wash Aer 35 wash Aer 40 wash
Figure 7 +e test results of wash durability for the treated fabrics (note A Escherichia coli B Staphylococcus aureus)
Table 9 Bacterial reduction test on the Pad-Dry-Cure treated fabric
was assessed for bacterial reduction test against Escherichiacoli and Staphylococcus aureus Maximum bacterial re-duction percentage was observed against Staphylococcusaureus and Escherichia coli when the wetting time was 30and 40minutes
Data Availability
+e authors have annotated the entire data building processthe empirical techniques presented in the paper and thenumber of runs generated using Design-Expert and Minitab18 software for optimization and analyzation based on theirparameters All data used to support the findings of thisstudy are included within the paper
Conflicts of Interest
Asnake Ketema is currently working as a lecturer in textilechemistry at Dire Dawa Institute of Technology Dire DawaUniversity Dire Dawa Ethiopia Amare Worku is cur-rently working as lecturer in textile chemistry and SchoolDean of the School of Textile Apparel and Fashion Designat Dire Dawa Institute of Technology Dire Dawa Uni-versity Dire Dawa Ethiopia +e authors declare that thereare no conflicts of interest regarding the publication of thispaper
Acknowledgments
+e authors would like to thank their advisor Dr GNalankilli professor of textile chemistry for his supportinvaluable guidance and constructive criticism during thesiswork and Dr Tamrat Tesfaye the secretary of the committeefor his encouragement and hard questions +is work wouldnot have been possible without the financial support of theEthiopian Institute of Textile and Fashion Technology(EiTEX) only for research work
References
[1] A Kalia B Joshi and M Mukhija ldquoPharmacognostical re-view of Urtica dioica Lrdquo International Journal of GreenPharmacy (IJGP) vol 8 no 4 pp 1998ndash4103 2014
[2] J Sheikh N Singh and M Srivastava ldquoFunctional dyeing ofcellulose-based (linen) fabric using Bombax ceiba (kapok)flower extractrdquo Fibers and Polymers vol 20 no 2 pp 312ndash319 2019
[3] L Qian ldquoApplication of nanotechnology for high perfor-mance textilesrdquo Journal of Textile and Apparel Technologyand Management vol 4 no 1 pp 1ndash7 2004
[4] C K Kang S S Kim S Kim et al ldquoAntibacterial cotton fiberstreated with silver nanoparticles and quaternary ammoniumsaltsrdquo Carbohydrate Polymers vol 151 pp 1012ndash1018 2016
[5] J E Herrera ldquoSynthesis of nanodispersed oxides of vanadiumtitanium molybdenum and tungsten on Mesoporous silicausing atomic layer depositionrdquo Topics in Catalysis vol 39no 3-4 pp 245ndash255 2006
[6] J Hudec M Burdova L u Kobida et al ldquoAntioxidant ca-pacity changes and phenolic profile of Echinacea purpureanettle (Urtica dioica L) and dandelion (Taraxacum officinale)after application of polyamine and phenolic biosynthesis
regulatorsrdquo Journal of Agricultural and Food Chemistryvol 55 no 14 pp 5689ndash5696 2007
[7] N A Ibrahim M H Abo-Shosha M A GaffarA M Elshafei and O M Abdel-Fatah ldquoAntibacterialproperties of ester-cross-linked cellulose-containing fabricspost-treated with metal saltsrdquo Polymer-Plastics Technologyand Engineering vol 45 no 6 pp 719ndash727 2006
[8] G +ilagavathi and S K Bala ldquoMicroencapsulation of herbalextracts for microbial resistance in healthcare textilesrdquoJournal of Fiber and Textile Research vol 32 no 1 pp 351ndash354 2007
[9] N A Salih ldquoAntibacterial effect of nettle (Urtica dioica)rdquo Al-Qadisiyah Journal of Veterinary Medicine Sciences vol 13no 1 p 1 2014
[10] K K Ghaima N M Hashim and S A Ali ldquoAntibacterial andantioxidant activities of ethyl acetate extract of nettle (Urticadioica) and dandelion (Taraxacum officinale)rdquo Journal ofApplied Pharmaceutical Science vol 3 no 5 p 96 2013
[11] T L Vigo Protection of Textiles from Biological AttackWoodhead Publishing Sawston UK 1st edition 2005
[12] S Hashemikia andMMontazer ldquoSodium hypophosphite andnano TiO2 inorganic catalysts along with citric acid on textileproducing multi-functional propertiesrdquo Applied Catalysis AGeneral vol 417-418 pp 200ndash208 2012
[13] M Montazer and M G Afjeh ldquoSimultaneous x-linking andantimicrobial finishing of cotton fabricrdquo Journal of AppliedPolymer Science vol 103 no 1 pp 178ndash185 2007
[14] R Aladpoosh and M Montazer ldquo+e role of cellulosic chainsof cotton in biosynthesis of ZnO nanorods producing mul-tifunctional properties mechanism characterizations andfeaturesrdquo Carbohydrate Polymers vol 126 pp 122ndash129 2015
[15] PS Vankar ldquoAntibacterial and antioxidant activities of ethylacetate extract of nettle (Urtica dioica) and dandelion (Tar-axacum officinale)rdquo Journal of Applied Pharmaceutical Sci-ence vol 3 pp 096ndash099 2013
[16] T Nithya J Jayanthi and M Ragunathan ldquoAntioxidantactivity total phenol flavonoid alkaloid tannin and saponincontents of leaf extracts of Salvinia molesta DS MitchellrdquoAsian Journal of Pharmaceutical and Clinical Research vol 9no 1 pp 200ndash203 2016
[17] R Roghini and K J Vijayalakshmi ldquoPhytochemical screen-ing quantitative analysis of flavonoids and minerals inethanolic extract of citrus paradisirdquo International Journal ofPharmaceutical Sciences and Research vol 9 no 11pp 4859ndash4864 2018
[18] F Sidaoui ldquoStudy of Tunisian nettle leaves (Urtica dioica L)mineral composition and antioxidant capacity of their ex-tracts obtained by maceration and supercritical fluid ex-tractionrdquo International Journal of Pharmacognosy andPhytochemical Research vol 7 pp 707ndash713 2015
[19] B Simoncic and B Tomsic ldquoStructures of novel antimicrobialagents for textiles-a reviewrdquo Textile Research Journal vol 80no 16 pp 1721ndash1737 2010
[20] G Sun and S D Worley ldquoChemistry of durable and re-generable biocidal textilesrdquo Journal of Chemical Educationvol 82 no 1 p 60 2005
[21] P Jaswal S AgyaPreet and G J Goel ldquoAntimicrobial activityof herbal treated cotton fabricrdquo International ResearchJournal of Engineering and Technology vol 4 no 8 pp 39ndash432017
[22] M Sathianarayanan ldquoAntibacterial finish for cotton fabricfrom herbal productsrdquo Indian Journal of Fiber and TextileResearch vol 35 pp 50ndash58 2010
Journal of Chemistry 9
[23] D Kut ldquoEffects of environmental conditions on the anti-bacterial activity of treated cotton knitsrdquo AATCC Reviewvol 5 no 3 2005
[24] N Afraz ldquoAntimicrobial finishes for textilesrdquo Including re-sults for Curr Trends Fashion Technology Textile Engineeringvol 5 p 4 2019
[25] A El-Shafei ldquoHerbal extract as an ecofriendly antibacterialfinishing of cotton fabricrdquo Egyptian Journal of Chemistryvol 61 no 2 pp 317ndash327 2018
[26] A Haji M Nasiriboroumand and S S Qavamnia ldquoCottondyeing and antibacterial finishing using agricultural waste byan eco-friendly process optimized by response surfacemethodologyrdquo Fibers and Polymers vol 19 no 11pp 2359ndash2364 2018
[27] A Reshma V B Priyadarisini and K Amutha ldquoSustainableantimicrobial finishing of fabrics using natural bioactiveagentsrdquo International Journal of Life Science vol 4 pp 10ndash202018
[28] W Ibrahim ldquoAloe vera leaf gel extract for antibacterial andsoftness properties of cottonrdquo Journal of Textile Science ampEngineering vol 7 no 301 p 2 2017
[29] P S Vankar R Shanker and S Wijayapala ldquoDyeing ofcotton wool and silk with extract of Allium cepardquo Pigment ampResin Technology vol 38 no 4 pp 242ndash247 2009
[30] G Singh ldquoFunctionalization of wool fabric using kapokflower and bio-mordantrdquo Sustainable Chemistry and Phar-macy vol 14 pp 2352ndash5541 2019
[31] K Gong Y Pan L J Rather et al ldquoNatural pigment duringflora leaf senescence and its application in dyeing and UVprotection finish of silk and woolmdasha case study of Cinna-momum camphorardquoDyes and Pigments vol 166 pp 114ndash1212019
[32] J Sheikh ldquoUltrasound assisted extraction of natural dyes andnatural mordants vis a vis dyeingrdquo Fibers and Polymersvol 17 no 5 pp 738ndash743 2016
[33] K Koszegi ldquoAntimicrobial Effects of the stinging nettle(Urtica dioica L)rdquo Analecta Technical Szegedinensia vol 11p 22 2017
[34] K Belay andM J C M R Sisay ldquoPhytochemical constituentsand physicochemical properties of medicinal plant (Moringaoleifera) around Bule Horardquo Chemistry and Materials Re-search vol 6 no 7 pp 61ndash72 2014
[35] K Murugesh Babu and K B Ravindra ldquoBioactive antimi-crobial agents for finishing of textiles for health care prod-uctsrdquo 4e Journal of the Textile Institute vol 106 no 7pp 706ndash717 2015
[36] I Gulccedilin ldquoAntioxidant antimicrobial antiulcer and analgesicactivities of nettle (Urtica dioica L)rdquo Journal of Ethno-pharmacology vol 90 no 2-3 pp 205ndash215 2004
[37] P Mantecca E Moschini P Bonfanti et al ldquoToxicity eval-uation of a new Zn-doped CuO nanocomposite with highlyeffective antibacterial propertiesrdquo Toxicological Sciencesvol 146 no 1 pp 16ndash30 2015
[38] V K Midha A Dakuri and V Midha ldquoStudies on theproperties of nonwoven surgical gownsrdquo Journal of IndustrialTextiles vol 43 no 2 pp 174ndash190 2013
[39] S W Ali S Rajendran and M Joshi ldquoSynthesis and char-acterization of chitosan and silver loaded chitosan nano-particles for bioactive polyesterrdquo Carbohydrate Polymersvol 83 no 2 pp 438ndash446 2011
[40] G M L Bearman A Rosato K Elam et al ldquoA crossover trialof antimicrobial scrubs to reduce methicillin-resistantStaphylococcus aureus burden on healthcare worker apparelrdquo
Infection Control amp Hospital Epidemiology vol 33 no 3pp 268ndash275 2012
[41] F Eser and A Onal ldquoDyeing of wool and cotton with extractof the nettle (Urtica dioica L) leavesrdquo Journal of NaturalFibers vol 12 no 3 pp 222ndash231 2015
[42] G Bag ldquoAssessment of total flavonoid content and antioxi-dant activity of methanolic rhizome extract of threeHedychium species of Manipur valleyrdquo International Journalof Pharmaceutical Sciences vol 30 no 1 pp 154ndash159 2015
[43] S ETHurovic ldquoChemical composition of stinging nettle leavesobtained by different analytical approachesrdquo Journal ofFunctional Food vol 32 pp 18ndash26 2017
[44] C S Ezeonu and C M Ejikeme ldquoQualitative and quantitativedetermination of phytochemical contents of indigenousNigerian softwoodsrdquo New Journal of Science vol 56 ArticleID 5601327 9 pages 2016
[45] H Y Fu S J Chen R F Chen W H Ding L L Kuo-Huangand R N Huang ldquoIdentification of oxalic acid and tartaricacid as major persistent pain-inducing toxins in the stinginghairs of the nettle Urtica thunbergianardquo Annals of Botanyvol 98 no 1 pp 57ndash65 2006
[46] Y Gao and R Cranston ldquoRecent advances in antimicrobialtreatments of textilesrdquo Textile Research Journal vol 78 no 1pp 60ndash72 2008
[47] S W Ali ldquoAntibacterial properties of aloe vera gel-finishedcotton fabricrdquo Cellulose vol 21 no 3 pp 2063ndash2072 2014
[48] M Gupta S +akur A Sharma and S Gupta ldquoQualitativeand quantitative analysis of phytochemicals and pharmaco-logical value of some dye yielding medicinal plantsrdquo OrientalJournal of Chemistry vol 29 no 2 pp 475ndash481 2013
10 Journal of Chemistry
210 Wash Durability Test +e treated fabrics were laun-dered using AATCC test method 61 Laundering was carriedout at MLR of 1 10 with 05 on weight of fabric of AATCCdetergent and 100 steel balls at a temperature of 90degC for 30minutes +e washing cycle was followed by hot rinsing inplain water at 40degC for 10 minutes Finally the washedswatches were tumble-dried Since a single wash-dry cyclesimulated 8 regular wash cycles the laundering procedurewas repeated 5 10 15 20 25 30 35 and 40 times to checkchemical durability
3 Results and Discussion
31 Yield of Extraction Using Water and Ethanol +e ex-perimental results (Table 2) can be illustrated by the fol-lowing linear equation
Yield 1015076 + 033 time + 0497487 conc (4)
Yield 1498065 + 031 Time + 0497487Conc (5)
Equations (4) and (5) depict the yield that has a linearrelationship with the factor of extraction time and con-centration of water and ethanol used as extraction solventrespectively
+e actual value and model prediction value of the yieldshowed a good correlation (Figure 2) Based on the ANOVAanalysis the linear equation has a p-value of 00001 (lt005)indicating that the equation model is significant
32 Analysis of Variance (ANOVA) +e results of theANOVA analysis factors A and B had a significant effect(Tables 3 and 4) +e factors A and B had a p-value of 00001and 00001 respectively +e model showed that the factorsA and B had a positive effect on the extraction yield indi-cating an increase in these factors extraction yield increases(Figure 3)
33 Optimization Extraction Parameters +e optimumconditions are based on the resulting desirability value +egoal of extraction is to minimize extraction time concen-tration and maximum water and ethanol extraction yield asshown in Tables 5 and 6 respectively +e optimizationprocess was performed by establishing the highest level ofextraction yield
Table 7 shows that the optimal extraction time is 59minutes with concentration of 10mlg the predictiveyield is 34991 percent Ethanolic extraction yield hasoptimal extraction time of 59026 minute with concen-tration of 10458mlg the predictive yield is 38716percent (Table 8)
34 Quantitative Analysis of Phytochemical Ingredients+e amount of total phenol content in the extract was de-termined by the Folin-Ciocalteau reagent described in theMaterials and Methods section using gallic acid as thestandard +e absorbance values obtained at differentconcentrations of gallic acid were used for the construction
of a calibration curve It appeared that the extraction ofnettle plant leaf total phenolic content is 27819plusmn 0131mgGAEg dry weight (equation (1))+e total flavonoid contentin the extract of nettle plant leaves is 2566plusmn 0227mgGAEgdry weight (equation (2)) [43ndash46]
FTIR studied in extracted nettle leaf displayed strongabsorption peaks at 307819 cmminus1 154929 cmminus1 140509 cmminus1and 107781 cmminus1 +e broad peak between 3500 cmminus1 and2500 cmminus1 corresponds to a strong O-H stretch vibrationwhich indicates the presence of hydroxyl groups in nettle leafextract On finger print region a doublet band is presentbetween1390 cmminus1 and 1310 cmminus1 representing O-H bendingwhich indicates phenolic compounds +e FTIR spectra of thetreated and untreated cotton fabric were almost the same andslight differences were at wave number 3000ndash2500 cmminus1 +etreated fabric has O-H stretch vibration and OH functionalgroup between 3000 and 2500 cmminus1 (Figure 4(a))
+e TGA curves of the crude extract showed that asmall weight loss was found in the range of 90ndash162degC dueto the evaporation of the humidity of the materials orvolatile compounds 162ndash537degC was associated with ali-phatic phenolic compounds decomposition or degrada-tion Char formation was detected between 537 and1028degC by further extending the analysis temperature(Figure 4(b))
35 Effect of Tensile Strength +e tensile strength of the Pad-Dry-Cure treated cotton fabric decreased by 066 and 117percent compared to the untreated control in warp and weftdirection respectively
Other physical properties such as permeability stiffnessstrength and absorbency were tested accordingly based onASTM ISO and AATCC standard respectively [33 47]
36 ReactionMechanisms +e two carboxylic groups of thecitric acid are linked with the hydroxyl part of the celluloseand with extracted phenol through covalent bond (Figure 5)+eir effective antibacterial activity and phenolic com-pounds were attached to cotton fabric using citric acid as acrosslinker Phenolic compounds are among the major anddiverse groups of active compounds in the nettle plant leafCotton fabrics treated with phenolic compounds showedexcellent antibacterial activity against the Gram-positivebacteria Staphylococcus aureus as well as the Gram-negativebacteria Escherichia coli
37AntibacterialActivity +e Pad-Dry-Cure treated fabricexhibited maximum antibacterial activity against Gram-negative test organisms compared to the Gram-positivetest organisms Maximum bacteria reduction was observedagainst Staphylococcus aureus and Escherichia coli whenthe padding mangle was applied at a pressure of 15 barwith 20 30 and 40 minutes of wetting time +is resultdemonstrated that the higher the wetting time (30 minutesand 40 minutes) in padding the better the antibacterialproperties At lower wetting time 20 minutes the anti-bacterial property is low as compared to the other wetting
Journal of Chemistry 5
Predicted vs actual
Color points by value ofyield25 55
30 35 40 504525 55Actual
25
30
35
40
45
50
55Pr
edic
ted
(a)
Color points by value ofyield29 59
Predicted vs actual
30 40 5020 60Actual
20
30
40
50
60
Pred
icte
d
(b)
Figure 2 Correlation between actual value and predicted value of (a) water and (b) ethanol extraction yield
Table 3 Analysis of variance (ANOVA) of the water extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 98997 2 49499 244408 lt00001
SignificantA time 79198 1 79198 391052 lt00001B conc 19799 1 19799 97763 lt00001Residual 203 10 02025Lack of fit 00253 6 00042 00084 10000 Not significantPure error 200 4 05000Cor total 99200 12
Table 4 Analysis of variance (ANOVA) of the ethanol extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 90780 2 45390 53341 lt00001
SignificantA time 70980 1 70980 83415 lt00001B conc 19799 1 19799 23268 lt00001Residual 851 10 08509Lack of fit 651 6 108 217 02367 Not significantPure error 200 4 05000Cor total 91631 12
Yield ()
Yiel
d (
)
55
50
45
40
35
30
25
25
20B concentration (mlg)
A time (m
inute)
1510 30
4050
6070
809030
Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
25 55
(a)
Yiel
d (
)
60
50
40
30
20
B concentration (mlg) A time (m
inute)25
2015
10 3040
5060
7080
9030
Yield ()Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
29 59
(b)
Figure 3 Interaction of factors time and temperature on (a) water and (b) ethanol extraction yield
Table 7 Optimization at minimum time concentration and high yield
Number Time (min) Conc(mlg) Yield () Desirability1 59896 10000 34991 0551 Selected
Table 8 Optimization at minimum time concentration and high yield
Number Time (min) Concentration (mlg) Yield Desirability1 59026 10458 38716 0547 Selected
008
006
004
002
000
4000 3500 3000 2500 2000Wave number (cmndash1)
1500 1000 500 0
Abso
rban
ce (
)
Untreated fabricTreated fabric dry
Powder extractedPowder
(a)
1000800600Temperature (degC)4002000
0
ndash5
ndash10
ndash15
ndash20
Mas
s los
s (m
g)
ndash25
ndash30
1200
(b)
Figure 4 Functional group and thermal analysis of nettle leaf extracted powder (a) combined FTIR spectra of untreated cotton fabric (b)thermography resulting from TGA analysis obtained under a nitrogen flow of 50mlmin and heating rate of 10degCmin
+
+
H
H C COOHH
H C C
O
O
OOC
HO C COOH
H
H
CHO
OH ndash celluloseCellulose
OH
RR R
R
RR
R
R
RR
C COOH
H
H
CCOOH
Citric acid Phenol derivatives
Figure 5 Mechanism of reaction between cellulose citric acid and phenolic compounds [48]
Journal of Chemistry 7
time +is effect could be becuase the longer the wettingtime of each particle of the extracted agents the deeper thepenetration inside the cotton fiber and the better thedurability (Table 9 Figure 6)
38 Durability to Laundering Generally the finishedscoured cotton fabric subjected to number of wash cycles (510 15 20 25 30 35 and 40) showed a gradual decrease inantibacterial property with 100 to 44 reduction in thebacterial count for Staphylococcus aureus and 100 to 30reduction in the bacterial count for Escherichia coli(Figure 7)
Citric acid as a crosslinking agent was added to theantibacterial finishing solutions It was found that the citric
acid was fairly effective against bacteria Adding poly-carboxylic acids to the antibacterial finishing recipes willenhance the durability of many laundering cycles
4 Conclusion
Natural and eco-friendly antibacterial finishing of textiles astrong antibacterial finishing of textile substrates withgood fastness and stability was obtained with nettle leafextract crosslinking on cotton fabrics using citric acid Itexhibits higher antibacterial efficiency +ere was a 100 to9975 percent reduction in the count of test bacteria afterPad-Dry-Cure treatment of the scoured cotton fabrics withthe dry nettle leaf extracted with optimized variables +eoptimization of the Pad-Dry-Cure conditions for finishing
S aureusSoaking time-20 minutes
S aureusSoaking time-30 minutes
S aureusSoaking time-40 minutes
E coliSoaking time-20 minutes
E coliSoaking time-30 minutes
E coliSoaking time-40 minutes
Figure 6 +e test results of Pad-Dry-Cure antibacterial treated fabric for Staphylococcus aureus and Escherichia coli
Aer 5 wash Aer 10 wash Aer 15 wash Aer 20 wash
Aer 25 wash Aer 30 wash Aer 35 wash Aer 40 wash
Figure 7 +e test results of wash durability for the treated fabrics (note A Escherichia coli B Staphylococcus aureus)
Table 9 Bacterial reduction test on the Pad-Dry-Cure treated fabric
was assessed for bacterial reduction test against Escherichiacoli and Staphylococcus aureus Maximum bacterial re-duction percentage was observed against Staphylococcusaureus and Escherichia coli when the wetting time was 30and 40minutes
Data Availability
+e authors have annotated the entire data building processthe empirical techniques presented in the paper and thenumber of runs generated using Design-Expert and Minitab18 software for optimization and analyzation based on theirparameters All data used to support the findings of thisstudy are included within the paper
Conflicts of Interest
Asnake Ketema is currently working as a lecturer in textilechemistry at Dire Dawa Institute of Technology Dire DawaUniversity Dire Dawa Ethiopia Amare Worku is cur-rently working as lecturer in textile chemistry and SchoolDean of the School of Textile Apparel and Fashion Designat Dire Dawa Institute of Technology Dire Dawa Uni-versity Dire Dawa Ethiopia +e authors declare that thereare no conflicts of interest regarding the publication of thispaper
Acknowledgments
+e authors would like to thank their advisor Dr GNalankilli professor of textile chemistry for his supportinvaluable guidance and constructive criticism during thesiswork and Dr Tamrat Tesfaye the secretary of the committeefor his encouragement and hard questions +is work wouldnot have been possible without the financial support of theEthiopian Institute of Textile and Fashion Technology(EiTEX) only for research work
References
[1] A Kalia B Joshi and M Mukhija ldquoPharmacognostical re-view of Urtica dioica Lrdquo International Journal of GreenPharmacy (IJGP) vol 8 no 4 pp 1998ndash4103 2014
[2] J Sheikh N Singh and M Srivastava ldquoFunctional dyeing ofcellulose-based (linen) fabric using Bombax ceiba (kapok)flower extractrdquo Fibers and Polymers vol 20 no 2 pp 312ndash319 2019
[3] L Qian ldquoApplication of nanotechnology for high perfor-mance textilesrdquo Journal of Textile and Apparel Technologyand Management vol 4 no 1 pp 1ndash7 2004
[4] C K Kang S S Kim S Kim et al ldquoAntibacterial cotton fiberstreated with silver nanoparticles and quaternary ammoniumsaltsrdquo Carbohydrate Polymers vol 151 pp 1012ndash1018 2016
[5] J E Herrera ldquoSynthesis of nanodispersed oxides of vanadiumtitanium molybdenum and tungsten on Mesoporous silicausing atomic layer depositionrdquo Topics in Catalysis vol 39no 3-4 pp 245ndash255 2006
[6] J Hudec M Burdova L u Kobida et al ldquoAntioxidant ca-pacity changes and phenolic profile of Echinacea purpureanettle (Urtica dioica L) and dandelion (Taraxacum officinale)after application of polyamine and phenolic biosynthesis
regulatorsrdquo Journal of Agricultural and Food Chemistryvol 55 no 14 pp 5689ndash5696 2007
[7] N A Ibrahim M H Abo-Shosha M A GaffarA M Elshafei and O M Abdel-Fatah ldquoAntibacterialproperties of ester-cross-linked cellulose-containing fabricspost-treated with metal saltsrdquo Polymer-Plastics Technologyand Engineering vol 45 no 6 pp 719ndash727 2006
[8] G +ilagavathi and S K Bala ldquoMicroencapsulation of herbalextracts for microbial resistance in healthcare textilesrdquoJournal of Fiber and Textile Research vol 32 no 1 pp 351ndash354 2007
[9] N A Salih ldquoAntibacterial effect of nettle (Urtica dioica)rdquo Al-Qadisiyah Journal of Veterinary Medicine Sciences vol 13no 1 p 1 2014
[10] K K Ghaima N M Hashim and S A Ali ldquoAntibacterial andantioxidant activities of ethyl acetate extract of nettle (Urticadioica) and dandelion (Taraxacum officinale)rdquo Journal ofApplied Pharmaceutical Science vol 3 no 5 p 96 2013
[11] T L Vigo Protection of Textiles from Biological AttackWoodhead Publishing Sawston UK 1st edition 2005
[12] S Hashemikia andMMontazer ldquoSodium hypophosphite andnano TiO2 inorganic catalysts along with citric acid on textileproducing multi-functional propertiesrdquo Applied Catalysis AGeneral vol 417-418 pp 200ndash208 2012
[13] M Montazer and M G Afjeh ldquoSimultaneous x-linking andantimicrobial finishing of cotton fabricrdquo Journal of AppliedPolymer Science vol 103 no 1 pp 178ndash185 2007
[14] R Aladpoosh and M Montazer ldquo+e role of cellulosic chainsof cotton in biosynthesis of ZnO nanorods producing mul-tifunctional properties mechanism characterizations andfeaturesrdquo Carbohydrate Polymers vol 126 pp 122ndash129 2015
[15] PS Vankar ldquoAntibacterial and antioxidant activities of ethylacetate extract of nettle (Urtica dioica) and dandelion (Tar-axacum officinale)rdquo Journal of Applied Pharmaceutical Sci-ence vol 3 pp 096ndash099 2013
[16] T Nithya J Jayanthi and M Ragunathan ldquoAntioxidantactivity total phenol flavonoid alkaloid tannin and saponincontents of leaf extracts of Salvinia molesta DS MitchellrdquoAsian Journal of Pharmaceutical and Clinical Research vol 9no 1 pp 200ndash203 2016
[17] R Roghini and K J Vijayalakshmi ldquoPhytochemical screen-ing quantitative analysis of flavonoids and minerals inethanolic extract of citrus paradisirdquo International Journal ofPharmaceutical Sciences and Research vol 9 no 11pp 4859ndash4864 2018
[18] F Sidaoui ldquoStudy of Tunisian nettle leaves (Urtica dioica L)mineral composition and antioxidant capacity of their ex-tracts obtained by maceration and supercritical fluid ex-tractionrdquo International Journal of Pharmacognosy andPhytochemical Research vol 7 pp 707ndash713 2015
[19] B Simoncic and B Tomsic ldquoStructures of novel antimicrobialagents for textiles-a reviewrdquo Textile Research Journal vol 80no 16 pp 1721ndash1737 2010
[20] G Sun and S D Worley ldquoChemistry of durable and re-generable biocidal textilesrdquo Journal of Chemical Educationvol 82 no 1 p 60 2005
[21] P Jaswal S AgyaPreet and G J Goel ldquoAntimicrobial activityof herbal treated cotton fabricrdquo International ResearchJournal of Engineering and Technology vol 4 no 8 pp 39ndash432017
[22] M Sathianarayanan ldquoAntibacterial finish for cotton fabricfrom herbal productsrdquo Indian Journal of Fiber and TextileResearch vol 35 pp 50ndash58 2010
Journal of Chemistry 9
[23] D Kut ldquoEffects of environmental conditions on the anti-bacterial activity of treated cotton knitsrdquo AATCC Reviewvol 5 no 3 2005
[24] N Afraz ldquoAntimicrobial finishes for textilesrdquo Including re-sults for Curr Trends Fashion Technology Textile Engineeringvol 5 p 4 2019
[25] A El-Shafei ldquoHerbal extract as an ecofriendly antibacterialfinishing of cotton fabricrdquo Egyptian Journal of Chemistryvol 61 no 2 pp 317ndash327 2018
[26] A Haji M Nasiriboroumand and S S Qavamnia ldquoCottondyeing and antibacterial finishing using agricultural waste byan eco-friendly process optimized by response surfacemethodologyrdquo Fibers and Polymers vol 19 no 11pp 2359ndash2364 2018
[27] A Reshma V B Priyadarisini and K Amutha ldquoSustainableantimicrobial finishing of fabrics using natural bioactiveagentsrdquo International Journal of Life Science vol 4 pp 10ndash202018
[28] W Ibrahim ldquoAloe vera leaf gel extract for antibacterial andsoftness properties of cottonrdquo Journal of Textile Science ampEngineering vol 7 no 301 p 2 2017
[29] P S Vankar R Shanker and S Wijayapala ldquoDyeing ofcotton wool and silk with extract of Allium cepardquo Pigment ampResin Technology vol 38 no 4 pp 242ndash247 2009
[30] G Singh ldquoFunctionalization of wool fabric using kapokflower and bio-mordantrdquo Sustainable Chemistry and Phar-macy vol 14 pp 2352ndash5541 2019
[31] K Gong Y Pan L J Rather et al ldquoNatural pigment duringflora leaf senescence and its application in dyeing and UVprotection finish of silk and woolmdasha case study of Cinna-momum camphorardquoDyes and Pigments vol 166 pp 114ndash1212019
[32] J Sheikh ldquoUltrasound assisted extraction of natural dyes andnatural mordants vis a vis dyeingrdquo Fibers and Polymersvol 17 no 5 pp 738ndash743 2016
[33] K Koszegi ldquoAntimicrobial Effects of the stinging nettle(Urtica dioica L)rdquo Analecta Technical Szegedinensia vol 11p 22 2017
[34] K Belay andM J C M R Sisay ldquoPhytochemical constituentsand physicochemical properties of medicinal plant (Moringaoleifera) around Bule Horardquo Chemistry and Materials Re-search vol 6 no 7 pp 61ndash72 2014
[35] K Murugesh Babu and K B Ravindra ldquoBioactive antimi-crobial agents for finishing of textiles for health care prod-uctsrdquo 4e Journal of the Textile Institute vol 106 no 7pp 706ndash717 2015
[36] I Gulccedilin ldquoAntioxidant antimicrobial antiulcer and analgesicactivities of nettle (Urtica dioica L)rdquo Journal of Ethno-pharmacology vol 90 no 2-3 pp 205ndash215 2004
[37] P Mantecca E Moschini P Bonfanti et al ldquoToxicity eval-uation of a new Zn-doped CuO nanocomposite with highlyeffective antibacterial propertiesrdquo Toxicological Sciencesvol 146 no 1 pp 16ndash30 2015
[38] V K Midha A Dakuri and V Midha ldquoStudies on theproperties of nonwoven surgical gownsrdquo Journal of IndustrialTextiles vol 43 no 2 pp 174ndash190 2013
[39] S W Ali S Rajendran and M Joshi ldquoSynthesis and char-acterization of chitosan and silver loaded chitosan nano-particles for bioactive polyesterrdquo Carbohydrate Polymersvol 83 no 2 pp 438ndash446 2011
[40] G M L Bearman A Rosato K Elam et al ldquoA crossover trialof antimicrobial scrubs to reduce methicillin-resistantStaphylococcus aureus burden on healthcare worker apparelrdquo
Infection Control amp Hospital Epidemiology vol 33 no 3pp 268ndash275 2012
[41] F Eser and A Onal ldquoDyeing of wool and cotton with extractof the nettle (Urtica dioica L) leavesrdquo Journal of NaturalFibers vol 12 no 3 pp 222ndash231 2015
[42] G Bag ldquoAssessment of total flavonoid content and antioxi-dant activity of methanolic rhizome extract of threeHedychium species of Manipur valleyrdquo International Journalof Pharmaceutical Sciences vol 30 no 1 pp 154ndash159 2015
[43] S ETHurovic ldquoChemical composition of stinging nettle leavesobtained by different analytical approachesrdquo Journal ofFunctional Food vol 32 pp 18ndash26 2017
[44] C S Ezeonu and C M Ejikeme ldquoQualitative and quantitativedetermination of phytochemical contents of indigenousNigerian softwoodsrdquo New Journal of Science vol 56 ArticleID 5601327 9 pages 2016
[45] H Y Fu S J Chen R F Chen W H Ding L L Kuo-Huangand R N Huang ldquoIdentification of oxalic acid and tartaricacid as major persistent pain-inducing toxins in the stinginghairs of the nettle Urtica thunbergianardquo Annals of Botanyvol 98 no 1 pp 57ndash65 2006
[46] Y Gao and R Cranston ldquoRecent advances in antimicrobialtreatments of textilesrdquo Textile Research Journal vol 78 no 1pp 60ndash72 2008
[47] S W Ali ldquoAntibacterial properties of aloe vera gel-finishedcotton fabricrdquo Cellulose vol 21 no 3 pp 2063ndash2072 2014
[48] M Gupta S +akur A Sharma and S Gupta ldquoQualitativeand quantitative analysis of phytochemicals and pharmaco-logical value of some dye yielding medicinal plantsrdquo OrientalJournal of Chemistry vol 29 no 2 pp 475ndash481 2013
10 Journal of Chemistry
Predicted vs actual
Color points by value ofyield25 55
30 35 40 504525 55Actual
25
30
35
40
45
50
55Pr
edic
ted
(a)
Color points by value ofyield29 59
Predicted vs actual
30 40 5020 60Actual
20
30
40
50
60
Pred
icte
d
(b)
Figure 2 Correlation between actual value and predicted value of (a) water and (b) ethanol extraction yield
Table 3 Analysis of variance (ANOVA) of the water extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 98997 2 49499 244408 lt00001
SignificantA time 79198 1 79198 391052 lt00001B conc 19799 1 19799 97763 lt00001Residual 203 10 02025Lack of fit 00253 6 00042 00084 10000 Not significantPure error 200 4 05000Cor total 99200 12
Table 4 Analysis of variance (ANOVA) of the ethanol extraction yield
Source Sum of squares DF Mean square F-value p-valueModel 90780 2 45390 53341 lt00001
SignificantA time 70980 1 70980 83415 lt00001B conc 19799 1 19799 23268 lt00001Residual 851 10 08509Lack of fit 651 6 108 217 02367 Not significantPure error 200 4 05000Cor total 91631 12
Yield ()
Yiel
d (
)
55
50
45
40
35
30
25
25
20B concentration (mlg)
A time (m
inute)
1510 30
4050
6070
809030
Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
25 55
(a)
Yiel
d (
)
60
50
40
30
20
B concentration (mlg) A time (m
inute)25
2015
10 3040
5060
7080
9030
Yield ()Design points abovepredicted valueDesign points belowpredicted value
X1 = A timeX2 = B concentration
29 59
(b)
Figure 3 Interaction of factors time and temperature on (a) water and (b) ethanol extraction yield
Table 7 Optimization at minimum time concentration and high yield
Number Time (min) Conc(mlg) Yield () Desirability1 59896 10000 34991 0551 Selected
Table 8 Optimization at minimum time concentration and high yield
Number Time (min) Concentration (mlg) Yield Desirability1 59026 10458 38716 0547 Selected
008
006
004
002
000
4000 3500 3000 2500 2000Wave number (cmndash1)
1500 1000 500 0
Abso
rban
ce (
)
Untreated fabricTreated fabric dry
Powder extractedPowder
(a)
1000800600Temperature (degC)4002000
0
ndash5
ndash10
ndash15
ndash20
Mas
s los
s (m
g)
ndash25
ndash30
1200
(b)
Figure 4 Functional group and thermal analysis of nettle leaf extracted powder (a) combined FTIR spectra of untreated cotton fabric (b)thermography resulting from TGA analysis obtained under a nitrogen flow of 50mlmin and heating rate of 10degCmin
+
+
H
H C COOHH
H C C
O
O
OOC
HO C COOH
H
H
CHO
OH ndash celluloseCellulose
OH
RR R
R
RR
R
R
RR
C COOH
H
H
CCOOH
Citric acid Phenol derivatives
Figure 5 Mechanism of reaction between cellulose citric acid and phenolic compounds [48]
Journal of Chemistry 7
time +is effect could be becuase the longer the wettingtime of each particle of the extracted agents the deeper thepenetration inside the cotton fiber and the better thedurability (Table 9 Figure 6)
38 Durability to Laundering Generally the finishedscoured cotton fabric subjected to number of wash cycles (510 15 20 25 30 35 and 40) showed a gradual decrease inantibacterial property with 100 to 44 reduction in thebacterial count for Staphylococcus aureus and 100 to 30reduction in the bacterial count for Escherichia coli(Figure 7)
Citric acid as a crosslinking agent was added to theantibacterial finishing solutions It was found that the citric
acid was fairly effective against bacteria Adding poly-carboxylic acids to the antibacterial finishing recipes willenhance the durability of many laundering cycles
4 Conclusion
Natural and eco-friendly antibacterial finishing of textiles astrong antibacterial finishing of textile substrates withgood fastness and stability was obtained with nettle leafextract crosslinking on cotton fabrics using citric acid Itexhibits higher antibacterial efficiency +ere was a 100 to9975 percent reduction in the count of test bacteria afterPad-Dry-Cure treatment of the scoured cotton fabrics withthe dry nettle leaf extracted with optimized variables +eoptimization of the Pad-Dry-Cure conditions for finishing
S aureusSoaking time-20 minutes
S aureusSoaking time-30 minutes
S aureusSoaking time-40 minutes
E coliSoaking time-20 minutes
E coliSoaking time-30 minutes
E coliSoaking time-40 minutes
Figure 6 +e test results of Pad-Dry-Cure antibacterial treated fabric for Staphylococcus aureus and Escherichia coli
Aer 5 wash Aer 10 wash Aer 15 wash Aer 20 wash
Aer 25 wash Aer 30 wash Aer 35 wash Aer 40 wash
Figure 7 +e test results of wash durability for the treated fabrics (note A Escherichia coli B Staphylococcus aureus)
Table 9 Bacterial reduction test on the Pad-Dry-Cure treated fabric
was assessed for bacterial reduction test against Escherichiacoli and Staphylococcus aureus Maximum bacterial re-duction percentage was observed against Staphylococcusaureus and Escherichia coli when the wetting time was 30and 40minutes
Data Availability
+e authors have annotated the entire data building processthe empirical techniques presented in the paper and thenumber of runs generated using Design-Expert and Minitab18 software for optimization and analyzation based on theirparameters All data used to support the findings of thisstudy are included within the paper
Conflicts of Interest
Asnake Ketema is currently working as a lecturer in textilechemistry at Dire Dawa Institute of Technology Dire DawaUniversity Dire Dawa Ethiopia Amare Worku is cur-rently working as lecturer in textile chemistry and SchoolDean of the School of Textile Apparel and Fashion Designat Dire Dawa Institute of Technology Dire Dawa Uni-versity Dire Dawa Ethiopia +e authors declare that thereare no conflicts of interest regarding the publication of thispaper
Acknowledgments
+e authors would like to thank their advisor Dr GNalankilli professor of textile chemistry for his supportinvaluable guidance and constructive criticism during thesiswork and Dr Tamrat Tesfaye the secretary of the committeefor his encouragement and hard questions +is work wouldnot have been possible without the financial support of theEthiopian Institute of Textile and Fashion Technology(EiTEX) only for research work
References
[1] A Kalia B Joshi and M Mukhija ldquoPharmacognostical re-view of Urtica dioica Lrdquo International Journal of GreenPharmacy (IJGP) vol 8 no 4 pp 1998ndash4103 2014
[2] J Sheikh N Singh and M Srivastava ldquoFunctional dyeing ofcellulose-based (linen) fabric using Bombax ceiba (kapok)flower extractrdquo Fibers and Polymers vol 20 no 2 pp 312ndash319 2019
[3] L Qian ldquoApplication of nanotechnology for high perfor-mance textilesrdquo Journal of Textile and Apparel Technologyand Management vol 4 no 1 pp 1ndash7 2004
[4] C K Kang S S Kim S Kim et al ldquoAntibacterial cotton fiberstreated with silver nanoparticles and quaternary ammoniumsaltsrdquo Carbohydrate Polymers vol 151 pp 1012ndash1018 2016
[5] J E Herrera ldquoSynthesis of nanodispersed oxides of vanadiumtitanium molybdenum and tungsten on Mesoporous silicausing atomic layer depositionrdquo Topics in Catalysis vol 39no 3-4 pp 245ndash255 2006
[6] J Hudec M Burdova L u Kobida et al ldquoAntioxidant ca-pacity changes and phenolic profile of Echinacea purpureanettle (Urtica dioica L) and dandelion (Taraxacum officinale)after application of polyamine and phenolic biosynthesis
regulatorsrdquo Journal of Agricultural and Food Chemistryvol 55 no 14 pp 5689ndash5696 2007
[7] N A Ibrahim M H Abo-Shosha M A GaffarA M Elshafei and O M Abdel-Fatah ldquoAntibacterialproperties of ester-cross-linked cellulose-containing fabricspost-treated with metal saltsrdquo Polymer-Plastics Technologyand Engineering vol 45 no 6 pp 719ndash727 2006
[8] G +ilagavathi and S K Bala ldquoMicroencapsulation of herbalextracts for microbial resistance in healthcare textilesrdquoJournal of Fiber and Textile Research vol 32 no 1 pp 351ndash354 2007
[9] N A Salih ldquoAntibacterial effect of nettle (Urtica dioica)rdquo Al-Qadisiyah Journal of Veterinary Medicine Sciences vol 13no 1 p 1 2014
[10] K K Ghaima N M Hashim and S A Ali ldquoAntibacterial andantioxidant activities of ethyl acetate extract of nettle (Urticadioica) and dandelion (Taraxacum officinale)rdquo Journal ofApplied Pharmaceutical Science vol 3 no 5 p 96 2013
[11] T L Vigo Protection of Textiles from Biological AttackWoodhead Publishing Sawston UK 1st edition 2005
[12] S Hashemikia andMMontazer ldquoSodium hypophosphite andnano TiO2 inorganic catalysts along with citric acid on textileproducing multi-functional propertiesrdquo Applied Catalysis AGeneral vol 417-418 pp 200ndash208 2012
[13] M Montazer and M G Afjeh ldquoSimultaneous x-linking andantimicrobial finishing of cotton fabricrdquo Journal of AppliedPolymer Science vol 103 no 1 pp 178ndash185 2007
[14] R Aladpoosh and M Montazer ldquo+e role of cellulosic chainsof cotton in biosynthesis of ZnO nanorods producing mul-tifunctional properties mechanism characterizations andfeaturesrdquo Carbohydrate Polymers vol 126 pp 122ndash129 2015
[15] PS Vankar ldquoAntibacterial and antioxidant activities of ethylacetate extract of nettle (Urtica dioica) and dandelion (Tar-axacum officinale)rdquo Journal of Applied Pharmaceutical Sci-ence vol 3 pp 096ndash099 2013
[16] T Nithya J Jayanthi and M Ragunathan ldquoAntioxidantactivity total phenol flavonoid alkaloid tannin and saponincontents of leaf extracts of Salvinia molesta DS MitchellrdquoAsian Journal of Pharmaceutical and Clinical Research vol 9no 1 pp 200ndash203 2016
[17] R Roghini and K J Vijayalakshmi ldquoPhytochemical screen-ing quantitative analysis of flavonoids and minerals inethanolic extract of citrus paradisirdquo International Journal ofPharmaceutical Sciences and Research vol 9 no 11pp 4859ndash4864 2018
[18] F Sidaoui ldquoStudy of Tunisian nettle leaves (Urtica dioica L)mineral composition and antioxidant capacity of their ex-tracts obtained by maceration and supercritical fluid ex-tractionrdquo International Journal of Pharmacognosy andPhytochemical Research vol 7 pp 707ndash713 2015
[19] B Simoncic and B Tomsic ldquoStructures of novel antimicrobialagents for textiles-a reviewrdquo Textile Research Journal vol 80no 16 pp 1721ndash1737 2010
[20] G Sun and S D Worley ldquoChemistry of durable and re-generable biocidal textilesrdquo Journal of Chemical Educationvol 82 no 1 p 60 2005
[21] P Jaswal S AgyaPreet and G J Goel ldquoAntimicrobial activityof herbal treated cotton fabricrdquo International ResearchJournal of Engineering and Technology vol 4 no 8 pp 39ndash432017
[22] M Sathianarayanan ldquoAntibacterial finish for cotton fabricfrom herbal productsrdquo Indian Journal of Fiber and TextileResearch vol 35 pp 50ndash58 2010
Journal of Chemistry 9
[23] D Kut ldquoEffects of environmental conditions on the anti-bacterial activity of treated cotton knitsrdquo AATCC Reviewvol 5 no 3 2005
[24] N Afraz ldquoAntimicrobial finishes for textilesrdquo Including re-sults for Curr Trends Fashion Technology Textile Engineeringvol 5 p 4 2019
[25] A El-Shafei ldquoHerbal extract as an ecofriendly antibacterialfinishing of cotton fabricrdquo Egyptian Journal of Chemistryvol 61 no 2 pp 317ndash327 2018
[26] A Haji M Nasiriboroumand and S S Qavamnia ldquoCottondyeing and antibacterial finishing using agricultural waste byan eco-friendly process optimized by response surfacemethodologyrdquo Fibers and Polymers vol 19 no 11pp 2359ndash2364 2018
[27] A Reshma V B Priyadarisini and K Amutha ldquoSustainableantimicrobial finishing of fabrics using natural bioactiveagentsrdquo International Journal of Life Science vol 4 pp 10ndash202018
[28] W Ibrahim ldquoAloe vera leaf gel extract for antibacterial andsoftness properties of cottonrdquo Journal of Textile Science ampEngineering vol 7 no 301 p 2 2017
[29] P S Vankar R Shanker and S Wijayapala ldquoDyeing ofcotton wool and silk with extract of Allium cepardquo Pigment ampResin Technology vol 38 no 4 pp 242ndash247 2009
[30] G Singh ldquoFunctionalization of wool fabric using kapokflower and bio-mordantrdquo Sustainable Chemistry and Phar-macy vol 14 pp 2352ndash5541 2019
[31] K Gong Y Pan L J Rather et al ldquoNatural pigment duringflora leaf senescence and its application in dyeing and UVprotection finish of silk and woolmdasha case study of Cinna-momum camphorardquoDyes and Pigments vol 166 pp 114ndash1212019
[32] J Sheikh ldquoUltrasound assisted extraction of natural dyes andnatural mordants vis a vis dyeingrdquo Fibers and Polymersvol 17 no 5 pp 738ndash743 2016
[33] K Koszegi ldquoAntimicrobial Effects of the stinging nettle(Urtica dioica L)rdquo Analecta Technical Szegedinensia vol 11p 22 2017
[34] K Belay andM J C M R Sisay ldquoPhytochemical constituentsand physicochemical properties of medicinal plant (Moringaoleifera) around Bule Horardquo Chemistry and Materials Re-search vol 6 no 7 pp 61ndash72 2014
[35] K Murugesh Babu and K B Ravindra ldquoBioactive antimi-crobial agents for finishing of textiles for health care prod-uctsrdquo 4e Journal of the Textile Institute vol 106 no 7pp 706ndash717 2015
[36] I Gulccedilin ldquoAntioxidant antimicrobial antiulcer and analgesicactivities of nettle (Urtica dioica L)rdquo Journal of Ethno-pharmacology vol 90 no 2-3 pp 205ndash215 2004
[37] P Mantecca E Moschini P Bonfanti et al ldquoToxicity eval-uation of a new Zn-doped CuO nanocomposite with highlyeffective antibacterial propertiesrdquo Toxicological Sciencesvol 146 no 1 pp 16ndash30 2015
[38] V K Midha A Dakuri and V Midha ldquoStudies on theproperties of nonwoven surgical gownsrdquo Journal of IndustrialTextiles vol 43 no 2 pp 174ndash190 2013
[39] S W Ali S Rajendran and M Joshi ldquoSynthesis and char-acterization of chitosan and silver loaded chitosan nano-particles for bioactive polyesterrdquo Carbohydrate Polymersvol 83 no 2 pp 438ndash446 2011
[40] G M L Bearman A Rosato K Elam et al ldquoA crossover trialof antimicrobial scrubs to reduce methicillin-resistantStaphylococcus aureus burden on healthcare worker apparelrdquo
Infection Control amp Hospital Epidemiology vol 33 no 3pp 268ndash275 2012
[41] F Eser and A Onal ldquoDyeing of wool and cotton with extractof the nettle (Urtica dioica L) leavesrdquo Journal of NaturalFibers vol 12 no 3 pp 222ndash231 2015
[42] G Bag ldquoAssessment of total flavonoid content and antioxi-dant activity of methanolic rhizome extract of threeHedychium species of Manipur valleyrdquo International Journalof Pharmaceutical Sciences vol 30 no 1 pp 154ndash159 2015
[43] S ETHurovic ldquoChemical composition of stinging nettle leavesobtained by different analytical approachesrdquo Journal ofFunctional Food vol 32 pp 18ndash26 2017
[44] C S Ezeonu and C M Ejikeme ldquoQualitative and quantitativedetermination of phytochemical contents of indigenousNigerian softwoodsrdquo New Journal of Science vol 56 ArticleID 5601327 9 pages 2016
[45] H Y Fu S J Chen R F Chen W H Ding L L Kuo-Huangand R N Huang ldquoIdentification of oxalic acid and tartaricacid as major persistent pain-inducing toxins in the stinginghairs of the nettle Urtica thunbergianardquo Annals of Botanyvol 98 no 1 pp 57ndash65 2006
[46] Y Gao and R Cranston ldquoRecent advances in antimicrobialtreatments of textilesrdquo Textile Research Journal vol 78 no 1pp 60ndash72 2008
[47] S W Ali ldquoAntibacterial properties of aloe vera gel-finishedcotton fabricrdquo Cellulose vol 21 no 3 pp 2063ndash2072 2014
[48] M Gupta S +akur A Sharma and S Gupta ldquoQualitativeand quantitative analysis of phytochemicals and pharmaco-logical value of some dye yielding medicinal plantsrdquo OrientalJournal of Chemistry vol 29 no 2 pp 475ndash481 2013
Table 7 Optimization at minimum time concentration and high yield
Number Time (min) Conc(mlg) Yield () Desirability1 59896 10000 34991 0551 Selected
Table 8 Optimization at minimum time concentration and high yield
Number Time (min) Concentration (mlg) Yield Desirability1 59026 10458 38716 0547 Selected
008
006
004
002
000
4000 3500 3000 2500 2000Wave number (cmndash1)
1500 1000 500 0
Abso
rban
ce (
)
Untreated fabricTreated fabric dry
Powder extractedPowder
(a)
1000800600Temperature (degC)4002000
0
ndash5
ndash10
ndash15
ndash20
Mas
s los
s (m
g)
ndash25
ndash30
1200
(b)
Figure 4 Functional group and thermal analysis of nettle leaf extracted powder (a) combined FTIR spectra of untreated cotton fabric (b)thermography resulting from TGA analysis obtained under a nitrogen flow of 50mlmin and heating rate of 10degCmin
+
+
H
H C COOHH
H C C
O
O
OOC
HO C COOH
H
H
CHO
OH ndash celluloseCellulose
OH
RR R
R
RR
R
R
RR
C COOH
H
H
CCOOH
Citric acid Phenol derivatives
Figure 5 Mechanism of reaction between cellulose citric acid and phenolic compounds [48]
Journal of Chemistry 7
time +is effect could be becuase the longer the wettingtime of each particle of the extracted agents the deeper thepenetration inside the cotton fiber and the better thedurability (Table 9 Figure 6)
38 Durability to Laundering Generally the finishedscoured cotton fabric subjected to number of wash cycles (510 15 20 25 30 35 and 40) showed a gradual decrease inantibacterial property with 100 to 44 reduction in thebacterial count for Staphylococcus aureus and 100 to 30reduction in the bacterial count for Escherichia coli(Figure 7)
Citric acid as a crosslinking agent was added to theantibacterial finishing solutions It was found that the citric
acid was fairly effective against bacteria Adding poly-carboxylic acids to the antibacterial finishing recipes willenhance the durability of many laundering cycles
4 Conclusion
Natural and eco-friendly antibacterial finishing of textiles astrong antibacterial finishing of textile substrates withgood fastness and stability was obtained with nettle leafextract crosslinking on cotton fabrics using citric acid Itexhibits higher antibacterial efficiency +ere was a 100 to9975 percent reduction in the count of test bacteria afterPad-Dry-Cure treatment of the scoured cotton fabrics withthe dry nettle leaf extracted with optimized variables +eoptimization of the Pad-Dry-Cure conditions for finishing
S aureusSoaking time-20 minutes
S aureusSoaking time-30 minutes
S aureusSoaking time-40 minutes
E coliSoaking time-20 minutes
E coliSoaking time-30 minutes
E coliSoaking time-40 minutes
Figure 6 +e test results of Pad-Dry-Cure antibacterial treated fabric for Staphylococcus aureus and Escherichia coli
Aer 5 wash Aer 10 wash Aer 15 wash Aer 20 wash
Aer 25 wash Aer 30 wash Aer 35 wash Aer 40 wash
Figure 7 +e test results of wash durability for the treated fabrics (note A Escherichia coli B Staphylococcus aureus)
Table 9 Bacterial reduction test on the Pad-Dry-Cure treated fabric
was assessed for bacterial reduction test against Escherichiacoli and Staphylococcus aureus Maximum bacterial re-duction percentage was observed against Staphylococcusaureus and Escherichia coli when the wetting time was 30and 40minutes
Data Availability
+e authors have annotated the entire data building processthe empirical techniques presented in the paper and thenumber of runs generated using Design-Expert and Minitab18 software for optimization and analyzation based on theirparameters All data used to support the findings of thisstudy are included within the paper
Conflicts of Interest
Asnake Ketema is currently working as a lecturer in textilechemistry at Dire Dawa Institute of Technology Dire DawaUniversity Dire Dawa Ethiopia Amare Worku is cur-rently working as lecturer in textile chemistry and SchoolDean of the School of Textile Apparel and Fashion Designat Dire Dawa Institute of Technology Dire Dawa Uni-versity Dire Dawa Ethiopia +e authors declare that thereare no conflicts of interest regarding the publication of thispaper
Acknowledgments
+e authors would like to thank their advisor Dr GNalankilli professor of textile chemistry for his supportinvaluable guidance and constructive criticism during thesiswork and Dr Tamrat Tesfaye the secretary of the committeefor his encouragement and hard questions +is work wouldnot have been possible without the financial support of theEthiopian Institute of Textile and Fashion Technology(EiTEX) only for research work
References
[1] A Kalia B Joshi and M Mukhija ldquoPharmacognostical re-view of Urtica dioica Lrdquo International Journal of GreenPharmacy (IJGP) vol 8 no 4 pp 1998ndash4103 2014
[2] J Sheikh N Singh and M Srivastava ldquoFunctional dyeing ofcellulose-based (linen) fabric using Bombax ceiba (kapok)flower extractrdquo Fibers and Polymers vol 20 no 2 pp 312ndash319 2019
[3] L Qian ldquoApplication of nanotechnology for high perfor-mance textilesrdquo Journal of Textile and Apparel Technologyand Management vol 4 no 1 pp 1ndash7 2004
[4] C K Kang S S Kim S Kim et al ldquoAntibacterial cotton fiberstreated with silver nanoparticles and quaternary ammoniumsaltsrdquo Carbohydrate Polymers vol 151 pp 1012ndash1018 2016
[5] J E Herrera ldquoSynthesis of nanodispersed oxides of vanadiumtitanium molybdenum and tungsten on Mesoporous silicausing atomic layer depositionrdquo Topics in Catalysis vol 39no 3-4 pp 245ndash255 2006
[6] J Hudec M Burdova L u Kobida et al ldquoAntioxidant ca-pacity changes and phenolic profile of Echinacea purpureanettle (Urtica dioica L) and dandelion (Taraxacum officinale)after application of polyamine and phenolic biosynthesis
regulatorsrdquo Journal of Agricultural and Food Chemistryvol 55 no 14 pp 5689ndash5696 2007
[7] N A Ibrahim M H Abo-Shosha M A GaffarA M Elshafei and O M Abdel-Fatah ldquoAntibacterialproperties of ester-cross-linked cellulose-containing fabricspost-treated with metal saltsrdquo Polymer-Plastics Technologyand Engineering vol 45 no 6 pp 719ndash727 2006
[8] G +ilagavathi and S K Bala ldquoMicroencapsulation of herbalextracts for microbial resistance in healthcare textilesrdquoJournal of Fiber and Textile Research vol 32 no 1 pp 351ndash354 2007
[9] N A Salih ldquoAntibacterial effect of nettle (Urtica dioica)rdquo Al-Qadisiyah Journal of Veterinary Medicine Sciences vol 13no 1 p 1 2014
[10] K K Ghaima N M Hashim and S A Ali ldquoAntibacterial andantioxidant activities of ethyl acetate extract of nettle (Urticadioica) and dandelion (Taraxacum officinale)rdquo Journal ofApplied Pharmaceutical Science vol 3 no 5 p 96 2013
[11] T L Vigo Protection of Textiles from Biological AttackWoodhead Publishing Sawston UK 1st edition 2005
[12] S Hashemikia andMMontazer ldquoSodium hypophosphite andnano TiO2 inorganic catalysts along with citric acid on textileproducing multi-functional propertiesrdquo Applied Catalysis AGeneral vol 417-418 pp 200ndash208 2012
[13] M Montazer and M G Afjeh ldquoSimultaneous x-linking andantimicrobial finishing of cotton fabricrdquo Journal of AppliedPolymer Science vol 103 no 1 pp 178ndash185 2007
[14] R Aladpoosh and M Montazer ldquo+e role of cellulosic chainsof cotton in biosynthesis of ZnO nanorods producing mul-tifunctional properties mechanism characterizations andfeaturesrdquo Carbohydrate Polymers vol 126 pp 122ndash129 2015
[15] PS Vankar ldquoAntibacterial and antioxidant activities of ethylacetate extract of nettle (Urtica dioica) and dandelion (Tar-axacum officinale)rdquo Journal of Applied Pharmaceutical Sci-ence vol 3 pp 096ndash099 2013
[16] T Nithya J Jayanthi and M Ragunathan ldquoAntioxidantactivity total phenol flavonoid alkaloid tannin and saponincontents of leaf extracts of Salvinia molesta DS MitchellrdquoAsian Journal of Pharmaceutical and Clinical Research vol 9no 1 pp 200ndash203 2016
[17] R Roghini and K J Vijayalakshmi ldquoPhytochemical screen-ing quantitative analysis of flavonoids and minerals inethanolic extract of citrus paradisirdquo International Journal ofPharmaceutical Sciences and Research vol 9 no 11pp 4859ndash4864 2018
[18] F Sidaoui ldquoStudy of Tunisian nettle leaves (Urtica dioica L)mineral composition and antioxidant capacity of their ex-tracts obtained by maceration and supercritical fluid ex-tractionrdquo International Journal of Pharmacognosy andPhytochemical Research vol 7 pp 707ndash713 2015
[19] B Simoncic and B Tomsic ldquoStructures of novel antimicrobialagents for textiles-a reviewrdquo Textile Research Journal vol 80no 16 pp 1721ndash1737 2010
[20] G Sun and S D Worley ldquoChemistry of durable and re-generable biocidal textilesrdquo Journal of Chemical Educationvol 82 no 1 p 60 2005
[21] P Jaswal S AgyaPreet and G J Goel ldquoAntimicrobial activityof herbal treated cotton fabricrdquo International ResearchJournal of Engineering and Technology vol 4 no 8 pp 39ndash432017
[22] M Sathianarayanan ldquoAntibacterial finish for cotton fabricfrom herbal productsrdquo Indian Journal of Fiber and TextileResearch vol 35 pp 50ndash58 2010
Journal of Chemistry 9
[23] D Kut ldquoEffects of environmental conditions on the anti-bacterial activity of treated cotton knitsrdquo AATCC Reviewvol 5 no 3 2005
[24] N Afraz ldquoAntimicrobial finishes for textilesrdquo Including re-sults for Curr Trends Fashion Technology Textile Engineeringvol 5 p 4 2019
[25] A El-Shafei ldquoHerbal extract as an ecofriendly antibacterialfinishing of cotton fabricrdquo Egyptian Journal of Chemistryvol 61 no 2 pp 317ndash327 2018
[26] A Haji M Nasiriboroumand and S S Qavamnia ldquoCottondyeing and antibacterial finishing using agricultural waste byan eco-friendly process optimized by response surfacemethodologyrdquo Fibers and Polymers vol 19 no 11pp 2359ndash2364 2018
[27] A Reshma V B Priyadarisini and K Amutha ldquoSustainableantimicrobial finishing of fabrics using natural bioactiveagentsrdquo International Journal of Life Science vol 4 pp 10ndash202018
[28] W Ibrahim ldquoAloe vera leaf gel extract for antibacterial andsoftness properties of cottonrdquo Journal of Textile Science ampEngineering vol 7 no 301 p 2 2017
[29] P S Vankar R Shanker and S Wijayapala ldquoDyeing ofcotton wool and silk with extract of Allium cepardquo Pigment ampResin Technology vol 38 no 4 pp 242ndash247 2009
[30] G Singh ldquoFunctionalization of wool fabric using kapokflower and bio-mordantrdquo Sustainable Chemistry and Phar-macy vol 14 pp 2352ndash5541 2019
[31] K Gong Y Pan L J Rather et al ldquoNatural pigment duringflora leaf senescence and its application in dyeing and UVprotection finish of silk and woolmdasha case study of Cinna-momum camphorardquoDyes and Pigments vol 166 pp 114ndash1212019
[32] J Sheikh ldquoUltrasound assisted extraction of natural dyes andnatural mordants vis a vis dyeingrdquo Fibers and Polymersvol 17 no 5 pp 738ndash743 2016
[33] K Koszegi ldquoAntimicrobial Effects of the stinging nettle(Urtica dioica L)rdquo Analecta Technical Szegedinensia vol 11p 22 2017
[34] K Belay andM J C M R Sisay ldquoPhytochemical constituentsand physicochemical properties of medicinal plant (Moringaoleifera) around Bule Horardquo Chemistry and Materials Re-search vol 6 no 7 pp 61ndash72 2014
[35] K Murugesh Babu and K B Ravindra ldquoBioactive antimi-crobial agents for finishing of textiles for health care prod-uctsrdquo 4e Journal of the Textile Institute vol 106 no 7pp 706ndash717 2015
[36] I Gulccedilin ldquoAntioxidant antimicrobial antiulcer and analgesicactivities of nettle (Urtica dioica L)rdquo Journal of Ethno-pharmacology vol 90 no 2-3 pp 205ndash215 2004
[37] P Mantecca E Moschini P Bonfanti et al ldquoToxicity eval-uation of a new Zn-doped CuO nanocomposite with highlyeffective antibacterial propertiesrdquo Toxicological Sciencesvol 146 no 1 pp 16ndash30 2015
[38] V K Midha A Dakuri and V Midha ldquoStudies on theproperties of nonwoven surgical gownsrdquo Journal of IndustrialTextiles vol 43 no 2 pp 174ndash190 2013
[39] S W Ali S Rajendran and M Joshi ldquoSynthesis and char-acterization of chitosan and silver loaded chitosan nano-particles for bioactive polyesterrdquo Carbohydrate Polymersvol 83 no 2 pp 438ndash446 2011
[40] G M L Bearman A Rosato K Elam et al ldquoA crossover trialof antimicrobial scrubs to reduce methicillin-resistantStaphylococcus aureus burden on healthcare worker apparelrdquo
Infection Control amp Hospital Epidemiology vol 33 no 3pp 268ndash275 2012
[41] F Eser and A Onal ldquoDyeing of wool and cotton with extractof the nettle (Urtica dioica L) leavesrdquo Journal of NaturalFibers vol 12 no 3 pp 222ndash231 2015
[42] G Bag ldquoAssessment of total flavonoid content and antioxi-dant activity of methanolic rhizome extract of threeHedychium species of Manipur valleyrdquo International Journalof Pharmaceutical Sciences vol 30 no 1 pp 154ndash159 2015
[43] S ETHurovic ldquoChemical composition of stinging nettle leavesobtained by different analytical approachesrdquo Journal ofFunctional Food vol 32 pp 18ndash26 2017
[44] C S Ezeonu and C M Ejikeme ldquoQualitative and quantitativedetermination of phytochemical contents of indigenousNigerian softwoodsrdquo New Journal of Science vol 56 ArticleID 5601327 9 pages 2016
[45] H Y Fu S J Chen R F Chen W H Ding L L Kuo-Huangand R N Huang ldquoIdentification of oxalic acid and tartaricacid as major persistent pain-inducing toxins in the stinginghairs of the nettle Urtica thunbergianardquo Annals of Botanyvol 98 no 1 pp 57ndash65 2006
[46] Y Gao and R Cranston ldquoRecent advances in antimicrobialtreatments of textilesrdquo Textile Research Journal vol 78 no 1pp 60ndash72 2008
[47] S W Ali ldquoAntibacterial properties of aloe vera gel-finishedcotton fabricrdquo Cellulose vol 21 no 3 pp 2063ndash2072 2014
[48] M Gupta S +akur A Sharma and S Gupta ldquoQualitativeand quantitative analysis of phytochemicals and pharmaco-logical value of some dye yielding medicinal plantsrdquo OrientalJournal of Chemistry vol 29 no 2 pp 475ndash481 2013
10 Journal of Chemistry
time +is effect could be becuase the longer the wettingtime of each particle of the extracted agents the deeper thepenetration inside the cotton fiber and the better thedurability (Table 9 Figure 6)
38 Durability to Laundering Generally the finishedscoured cotton fabric subjected to number of wash cycles (510 15 20 25 30 35 and 40) showed a gradual decrease inantibacterial property with 100 to 44 reduction in thebacterial count for Staphylococcus aureus and 100 to 30reduction in the bacterial count for Escherichia coli(Figure 7)
Citric acid as a crosslinking agent was added to theantibacterial finishing solutions It was found that the citric
acid was fairly effective against bacteria Adding poly-carboxylic acids to the antibacterial finishing recipes willenhance the durability of many laundering cycles
4 Conclusion
Natural and eco-friendly antibacterial finishing of textiles astrong antibacterial finishing of textile substrates withgood fastness and stability was obtained with nettle leafextract crosslinking on cotton fabrics using citric acid Itexhibits higher antibacterial efficiency +ere was a 100 to9975 percent reduction in the count of test bacteria afterPad-Dry-Cure treatment of the scoured cotton fabrics withthe dry nettle leaf extracted with optimized variables +eoptimization of the Pad-Dry-Cure conditions for finishing
S aureusSoaking time-20 minutes
S aureusSoaking time-30 minutes
S aureusSoaking time-40 minutes
E coliSoaking time-20 minutes
E coliSoaking time-30 minutes
E coliSoaking time-40 minutes
Figure 6 +e test results of Pad-Dry-Cure antibacterial treated fabric for Staphylococcus aureus and Escherichia coli
Aer 5 wash Aer 10 wash Aer 15 wash Aer 20 wash
Aer 25 wash Aer 30 wash Aer 35 wash Aer 40 wash
Figure 7 +e test results of wash durability for the treated fabrics (note A Escherichia coli B Staphylococcus aureus)
Table 9 Bacterial reduction test on the Pad-Dry-Cure treated fabric
was assessed for bacterial reduction test against Escherichiacoli and Staphylococcus aureus Maximum bacterial re-duction percentage was observed against Staphylococcusaureus and Escherichia coli when the wetting time was 30and 40minutes
Data Availability
+e authors have annotated the entire data building processthe empirical techniques presented in the paper and thenumber of runs generated using Design-Expert and Minitab18 software for optimization and analyzation based on theirparameters All data used to support the findings of thisstudy are included within the paper
Conflicts of Interest
Asnake Ketema is currently working as a lecturer in textilechemistry at Dire Dawa Institute of Technology Dire DawaUniversity Dire Dawa Ethiopia Amare Worku is cur-rently working as lecturer in textile chemistry and SchoolDean of the School of Textile Apparel and Fashion Designat Dire Dawa Institute of Technology Dire Dawa Uni-versity Dire Dawa Ethiopia +e authors declare that thereare no conflicts of interest regarding the publication of thispaper
Acknowledgments
+e authors would like to thank their advisor Dr GNalankilli professor of textile chemistry for his supportinvaluable guidance and constructive criticism during thesiswork and Dr Tamrat Tesfaye the secretary of the committeefor his encouragement and hard questions +is work wouldnot have been possible without the financial support of theEthiopian Institute of Textile and Fashion Technology(EiTEX) only for research work
References
[1] A Kalia B Joshi and M Mukhija ldquoPharmacognostical re-view of Urtica dioica Lrdquo International Journal of GreenPharmacy (IJGP) vol 8 no 4 pp 1998ndash4103 2014
[2] J Sheikh N Singh and M Srivastava ldquoFunctional dyeing ofcellulose-based (linen) fabric using Bombax ceiba (kapok)flower extractrdquo Fibers and Polymers vol 20 no 2 pp 312ndash319 2019
[3] L Qian ldquoApplication of nanotechnology for high perfor-mance textilesrdquo Journal of Textile and Apparel Technologyand Management vol 4 no 1 pp 1ndash7 2004
[4] C K Kang S S Kim S Kim et al ldquoAntibacterial cotton fiberstreated with silver nanoparticles and quaternary ammoniumsaltsrdquo Carbohydrate Polymers vol 151 pp 1012ndash1018 2016
[5] J E Herrera ldquoSynthesis of nanodispersed oxides of vanadiumtitanium molybdenum and tungsten on Mesoporous silicausing atomic layer depositionrdquo Topics in Catalysis vol 39no 3-4 pp 245ndash255 2006
[6] J Hudec M Burdova L u Kobida et al ldquoAntioxidant ca-pacity changes and phenolic profile of Echinacea purpureanettle (Urtica dioica L) and dandelion (Taraxacum officinale)after application of polyamine and phenolic biosynthesis
regulatorsrdquo Journal of Agricultural and Food Chemistryvol 55 no 14 pp 5689ndash5696 2007
[7] N A Ibrahim M H Abo-Shosha M A GaffarA M Elshafei and O M Abdel-Fatah ldquoAntibacterialproperties of ester-cross-linked cellulose-containing fabricspost-treated with metal saltsrdquo Polymer-Plastics Technologyand Engineering vol 45 no 6 pp 719ndash727 2006
[8] G +ilagavathi and S K Bala ldquoMicroencapsulation of herbalextracts for microbial resistance in healthcare textilesrdquoJournal of Fiber and Textile Research vol 32 no 1 pp 351ndash354 2007
[9] N A Salih ldquoAntibacterial effect of nettle (Urtica dioica)rdquo Al-Qadisiyah Journal of Veterinary Medicine Sciences vol 13no 1 p 1 2014
[10] K K Ghaima N M Hashim and S A Ali ldquoAntibacterial andantioxidant activities of ethyl acetate extract of nettle (Urticadioica) and dandelion (Taraxacum officinale)rdquo Journal ofApplied Pharmaceutical Science vol 3 no 5 p 96 2013
[11] T L Vigo Protection of Textiles from Biological AttackWoodhead Publishing Sawston UK 1st edition 2005
[12] S Hashemikia andMMontazer ldquoSodium hypophosphite andnano TiO2 inorganic catalysts along with citric acid on textileproducing multi-functional propertiesrdquo Applied Catalysis AGeneral vol 417-418 pp 200ndash208 2012
[13] M Montazer and M G Afjeh ldquoSimultaneous x-linking andantimicrobial finishing of cotton fabricrdquo Journal of AppliedPolymer Science vol 103 no 1 pp 178ndash185 2007
[14] R Aladpoosh and M Montazer ldquo+e role of cellulosic chainsof cotton in biosynthesis of ZnO nanorods producing mul-tifunctional properties mechanism characterizations andfeaturesrdquo Carbohydrate Polymers vol 126 pp 122ndash129 2015
[15] PS Vankar ldquoAntibacterial and antioxidant activities of ethylacetate extract of nettle (Urtica dioica) and dandelion (Tar-axacum officinale)rdquo Journal of Applied Pharmaceutical Sci-ence vol 3 pp 096ndash099 2013
[16] T Nithya J Jayanthi and M Ragunathan ldquoAntioxidantactivity total phenol flavonoid alkaloid tannin and saponincontents of leaf extracts of Salvinia molesta DS MitchellrdquoAsian Journal of Pharmaceutical and Clinical Research vol 9no 1 pp 200ndash203 2016
[17] R Roghini and K J Vijayalakshmi ldquoPhytochemical screen-ing quantitative analysis of flavonoids and minerals inethanolic extract of citrus paradisirdquo International Journal ofPharmaceutical Sciences and Research vol 9 no 11pp 4859ndash4864 2018
[18] F Sidaoui ldquoStudy of Tunisian nettle leaves (Urtica dioica L)mineral composition and antioxidant capacity of their ex-tracts obtained by maceration and supercritical fluid ex-tractionrdquo International Journal of Pharmacognosy andPhytochemical Research vol 7 pp 707ndash713 2015
[19] B Simoncic and B Tomsic ldquoStructures of novel antimicrobialagents for textiles-a reviewrdquo Textile Research Journal vol 80no 16 pp 1721ndash1737 2010
[20] G Sun and S D Worley ldquoChemistry of durable and re-generable biocidal textilesrdquo Journal of Chemical Educationvol 82 no 1 p 60 2005
[21] P Jaswal S AgyaPreet and G J Goel ldquoAntimicrobial activityof herbal treated cotton fabricrdquo International ResearchJournal of Engineering and Technology vol 4 no 8 pp 39ndash432017
[22] M Sathianarayanan ldquoAntibacterial finish for cotton fabricfrom herbal productsrdquo Indian Journal of Fiber and TextileResearch vol 35 pp 50ndash58 2010
Journal of Chemistry 9
[23] D Kut ldquoEffects of environmental conditions on the anti-bacterial activity of treated cotton knitsrdquo AATCC Reviewvol 5 no 3 2005
[24] N Afraz ldquoAntimicrobial finishes for textilesrdquo Including re-sults for Curr Trends Fashion Technology Textile Engineeringvol 5 p 4 2019
[25] A El-Shafei ldquoHerbal extract as an ecofriendly antibacterialfinishing of cotton fabricrdquo Egyptian Journal of Chemistryvol 61 no 2 pp 317ndash327 2018
[26] A Haji M Nasiriboroumand and S S Qavamnia ldquoCottondyeing and antibacterial finishing using agricultural waste byan eco-friendly process optimized by response surfacemethodologyrdquo Fibers and Polymers vol 19 no 11pp 2359ndash2364 2018
[27] A Reshma V B Priyadarisini and K Amutha ldquoSustainableantimicrobial finishing of fabrics using natural bioactiveagentsrdquo International Journal of Life Science vol 4 pp 10ndash202018
[28] W Ibrahim ldquoAloe vera leaf gel extract for antibacterial andsoftness properties of cottonrdquo Journal of Textile Science ampEngineering vol 7 no 301 p 2 2017
[29] P S Vankar R Shanker and S Wijayapala ldquoDyeing ofcotton wool and silk with extract of Allium cepardquo Pigment ampResin Technology vol 38 no 4 pp 242ndash247 2009
[30] G Singh ldquoFunctionalization of wool fabric using kapokflower and bio-mordantrdquo Sustainable Chemistry and Phar-macy vol 14 pp 2352ndash5541 2019
[31] K Gong Y Pan L J Rather et al ldquoNatural pigment duringflora leaf senescence and its application in dyeing and UVprotection finish of silk and woolmdasha case study of Cinna-momum camphorardquoDyes and Pigments vol 166 pp 114ndash1212019
[32] J Sheikh ldquoUltrasound assisted extraction of natural dyes andnatural mordants vis a vis dyeingrdquo Fibers and Polymersvol 17 no 5 pp 738ndash743 2016
[33] K Koszegi ldquoAntimicrobial Effects of the stinging nettle(Urtica dioica L)rdquo Analecta Technical Szegedinensia vol 11p 22 2017
[34] K Belay andM J C M R Sisay ldquoPhytochemical constituentsand physicochemical properties of medicinal plant (Moringaoleifera) around Bule Horardquo Chemistry and Materials Re-search vol 6 no 7 pp 61ndash72 2014
[35] K Murugesh Babu and K B Ravindra ldquoBioactive antimi-crobial agents for finishing of textiles for health care prod-uctsrdquo 4e Journal of the Textile Institute vol 106 no 7pp 706ndash717 2015
[36] I Gulccedilin ldquoAntioxidant antimicrobial antiulcer and analgesicactivities of nettle (Urtica dioica L)rdquo Journal of Ethno-pharmacology vol 90 no 2-3 pp 205ndash215 2004
[37] P Mantecca E Moschini P Bonfanti et al ldquoToxicity eval-uation of a new Zn-doped CuO nanocomposite with highlyeffective antibacterial propertiesrdquo Toxicological Sciencesvol 146 no 1 pp 16ndash30 2015
[38] V K Midha A Dakuri and V Midha ldquoStudies on theproperties of nonwoven surgical gownsrdquo Journal of IndustrialTextiles vol 43 no 2 pp 174ndash190 2013
[39] S W Ali S Rajendran and M Joshi ldquoSynthesis and char-acterization of chitosan and silver loaded chitosan nano-particles for bioactive polyesterrdquo Carbohydrate Polymersvol 83 no 2 pp 438ndash446 2011
[40] G M L Bearman A Rosato K Elam et al ldquoA crossover trialof antimicrobial scrubs to reduce methicillin-resistantStaphylococcus aureus burden on healthcare worker apparelrdquo
Infection Control amp Hospital Epidemiology vol 33 no 3pp 268ndash275 2012
[41] F Eser and A Onal ldquoDyeing of wool and cotton with extractof the nettle (Urtica dioica L) leavesrdquo Journal of NaturalFibers vol 12 no 3 pp 222ndash231 2015
[42] G Bag ldquoAssessment of total flavonoid content and antioxi-dant activity of methanolic rhizome extract of threeHedychium species of Manipur valleyrdquo International Journalof Pharmaceutical Sciences vol 30 no 1 pp 154ndash159 2015
[43] S ETHurovic ldquoChemical composition of stinging nettle leavesobtained by different analytical approachesrdquo Journal ofFunctional Food vol 32 pp 18ndash26 2017
[44] C S Ezeonu and C M Ejikeme ldquoQualitative and quantitativedetermination of phytochemical contents of indigenousNigerian softwoodsrdquo New Journal of Science vol 56 ArticleID 5601327 9 pages 2016
[45] H Y Fu S J Chen R F Chen W H Ding L L Kuo-Huangand R N Huang ldquoIdentification of oxalic acid and tartaricacid as major persistent pain-inducing toxins in the stinginghairs of the nettle Urtica thunbergianardquo Annals of Botanyvol 98 no 1 pp 57ndash65 2006
[46] Y Gao and R Cranston ldquoRecent advances in antimicrobialtreatments of textilesrdquo Textile Research Journal vol 78 no 1pp 60ndash72 2008
[47] S W Ali ldquoAntibacterial properties of aloe vera gel-finishedcotton fabricrdquo Cellulose vol 21 no 3 pp 2063ndash2072 2014
[48] M Gupta S +akur A Sharma and S Gupta ldquoQualitativeand quantitative analysis of phytochemicals and pharmaco-logical value of some dye yielding medicinal plantsrdquo OrientalJournal of Chemistry vol 29 no 2 pp 475ndash481 2013
10 Journal of Chemistry
was assessed for bacterial reduction test against Escherichiacoli and Staphylococcus aureus Maximum bacterial re-duction percentage was observed against Staphylococcusaureus and Escherichia coli when the wetting time was 30and 40minutes
Data Availability
+e authors have annotated the entire data building processthe empirical techniques presented in the paper and thenumber of runs generated using Design-Expert and Minitab18 software for optimization and analyzation based on theirparameters All data used to support the findings of thisstudy are included within the paper
Conflicts of Interest
Asnake Ketema is currently working as a lecturer in textilechemistry at Dire Dawa Institute of Technology Dire DawaUniversity Dire Dawa Ethiopia Amare Worku is cur-rently working as lecturer in textile chemistry and SchoolDean of the School of Textile Apparel and Fashion Designat Dire Dawa Institute of Technology Dire Dawa Uni-versity Dire Dawa Ethiopia +e authors declare that thereare no conflicts of interest regarding the publication of thispaper
Acknowledgments
+e authors would like to thank their advisor Dr GNalankilli professor of textile chemistry for his supportinvaluable guidance and constructive criticism during thesiswork and Dr Tamrat Tesfaye the secretary of the committeefor his encouragement and hard questions +is work wouldnot have been possible without the financial support of theEthiopian Institute of Textile and Fashion Technology(EiTEX) only for research work
References
[1] A Kalia B Joshi and M Mukhija ldquoPharmacognostical re-view of Urtica dioica Lrdquo International Journal of GreenPharmacy (IJGP) vol 8 no 4 pp 1998ndash4103 2014
[2] J Sheikh N Singh and M Srivastava ldquoFunctional dyeing ofcellulose-based (linen) fabric using Bombax ceiba (kapok)flower extractrdquo Fibers and Polymers vol 20 no 2 pp 312ndash319 2019
[3] L Qian ldquoApplication of nanotechnology for high perfor-mance textilesrdquo Journal of Textile and Apparel Technologyand Management vol 4 no 1 pp 1ndash7 2004
[4] C K Kang S S Kim S Kim et al ldquoAntibacterial cotton fiberstreated with silver nanoparticles and quaternary ammoniumsaltsrdquo Carbohydrate Polymers vol 151 pp 1012ndash1018 2016
[5] J E Herrera ldquoSynthesis of nanodispersed oxides of vanadiumtitanium molybdenum and tungsten on Mesoporous silicausing atomic layer depositionrdquo Topics in Catalysis vol 39no 3-4 pp 245ndash255 2006
[6] J Hudec M Burdova L u Kobida et al ldquoAntioxidant ca-pacity changes and phenolic profile of Echinacea purpureanettle (Urtica dioica L) and dandelion (Taraxacum officinale)after application of polyamine and phenolic biosynthesis
regulatorsrdquo Journal of Agricultural and Food Chemistryvol 55 no 14 pp 5689ndash5696 2007
[7] N A Ibrahim M H Abo-Shosha M A GaffarA M Elshafei and O M Abdel-Fatah ldquoAntibacterialproperties of ester-cross-linked cellulose-containing fabricspost-treated with metal saltsrdquo Polymer-Plastics Technologyand Engineering vol 45 no 6 pp 719ndash727 2006
[8] G +ilagavathi and S K Bala ldquoMicroencapsulation of herbalextracts for microbial resistance in healthcare textilesrdquoJournal of Fiber and Textile Research vol 32 no 1 pp 351ndash354 2007
[9] N A Salih ldquoAntibacterial effect of nettle (Urtica dioica)rdquo Al-Qadisiyah Journal of Veterinary Medicine Sciences vol 13no 1 p 1 2014
[10] K K Ghaima N M Hashim and S A Ali ldquoAntibacterial andantioxidant activities of ethyl acetate extract of nettle (Urticadioica) and dandelion (Taraxacum officinale)rdquo Journal ofApplied Pharmaceutical Science vol 3 no 5 p 96 2013
[11] T L Vigo Protection of Textiles from Biological AttackWoodhead Publishing Sawston UK 1st edition 2005
[12] S Hashemikia andMMontazer ldquoSodium hypophosphite andnano TiO2 inorganic catalysts along with citric acid on textileproducing multi-functional propertiesrdquo Applied Catalysis AGeneral vol 417-418 pp 200ndash208 2012
[13] M Montazer and M G Afjeh ldquoSimultaneous x-linking andantimicrobial finishing of cotton fabricrdquo Journal of AppliedPolymer Science vol 103 no 1 pp 178ndash185 2007
[14] R Aladpoosh and M Montazer ldquo+e role of cellulosic chainsof cotton in biosynthesis of ZnO nanorods producing mul-tifunctional properties mechanism characterizations andfeaturesrdquo Carbohydrate Polymers vol 126 pp 122ndash129 2015
[15] PS Vankar ldquoAntibacterial and antioxidant activities of ethylacetate extract of nettle (Urtica dioica) and dandelion (Tar-axacum officinale)rdquo Journal of Applied Pharmaceutical Sci-ence vol 3 pp 096ndash099 2013
[16] T Nithya J Jayanthi and M Ragunathan ldquoAntioxidantactivity total phenol flavonoid alkaloid tannin and saponincontents of leaf extracts of Salvinia molesta DS MitchellrdquoAsian Journal of Pharmaceutical and Clinical Research vol 9no 1 pp 200ndash203 2016
[17] R Roghini and K J Vijayalakshmi ldquoPhytochemical screen-ing quantitative analysis of flavonoids and minerals inethanolic extract of citrus paradisirdquo International Journal ofPharmaceutical Sciences and Research vol 9 no 11pp 4859ndash4864 2018
[18] F Sidaoui ldquoStudy of Tunisian nettle leaves (Urtica dioica L)mineral composition and antioxidant capacity of their ex-tracts obtained by maceration and supercritical fluid ex-tractionrdquo International Journal of Pharmacognosy andPhytochemical Research vol 7 pp 707ndash713 2015
[19] B Simoncic and B Tomsic ldquoStructures of novel antimicrobialagents for textiles-a reviewrdquo Textile Research Journal vol 80no 16 pp 1721ndash1737 2010
[20] G Sun and S D Worley ldquoChemistry of durable and re-generable biocidal textilesrdquo Journal of Chemical Educationvol 82 no 1 p 60 2005
[21] P Jaswal S AgyaPreet and G J Goel ldquoAntimicrobial activityof herbal treated cotton fabricrdquo International ResearchJournal of Engineering and Technology vol 4 no 8 pp 39ndash432017
[22] M Sathianarayanan ldquoAntibacterial finish for cotton fabricfrom herbal productsrdquo Indian Journal of Fiber and TextileResearch vol 35 pp 50ndash58 2010
Journal of Chemistry 9
[23] D Kut ldquoEffects of environmental conditions on the anti-bacterial activity of treated cotton knitsrdquo AATCC Reviewvol 5 no 3 2005
[24] N Afraz ldquoAntimicrobial finishes for textilesrdquo Including re-sults for Curr Trends Fashion Technology Textile Engineeringvol 5 p 4 2019
[25] A El-Shafei ldquoHerbal extract as an ecofriendly antibacterialfinishing of cotton fabricrdquo Egyptian Journal of Chemistryvol 61 no 2 pp 317ndash327 2018
[26] A Haji M Nasiriboroumand and S S Qavamnia ldquoCottondyeing and antibacterial finishing using agricultural waste byan eco-friendly process optimized by response surfacemethodologyrdquo Fibers and Polymers vol 19 no 11pp 2359ndash2364 2018
[27] A Reshma V B Priyadarisini and K Amutha ldquoSustainableantimicrobial finishing of fabrics using natural bioactiveagentsrdquo International Journal of Life Science vol 4 pp 10ndash202018
[28] W Ibrahim ldquoAloe vera leaf gel extract for antibacterial andsoftness properties of cottonrdquo Journal of Textile Science ampEngineering vol 7 no 301 p 2 2017
[29] P S Vankar R Shanker and S Wijayapala ldquoDyeing ofcotton wool and silk with extract of Allium cepardquo Pigment ampResin Technology vol 38 no 4 pp 242ndash247 2009
[30] G Singh ldquoFunctionalization of wool fabric using kapokflower and bio-mordantrdquo Sustainable Chemistry and Phar-macy vol 14 pp 2352ndash5541 2019
[31] K Gong Y Pan L J Rather et al ldquoNatural pigment duringflora leaf senescence and its application in dyeing and UVprotection finish of silk and woolmdasha case study of Cinna-momum camphorardquoDyes and Pigments vol 166 pp 114ndash1212019
[32] J Sheikh ldquoUltrasound assisted extraction of natural dyes andnatural mordants vis a vis dyeingrdquo Fibers and Polymersvol 17 no 5 pp 738ndash743 2016
[33] K Koszegi ldquoAntimicrobial Effects of the stinging nettle(Urtica dioica L)rdquo Analecta Technical Szegedinensia vol 11p 22 2017
[34] K Belay andM J C M R Sisay ldquoPhytochemical constituentsand physicochemical properties of medicinal plant (Moringaoleifera) around Bule Horardquo Chemistry and Materials Re-search vol 6 no 7 pp 61ndash72 2014
[35] K Murugesh Babu and K B Ravindra ldquoBioactive antimi-crobial agents for finishing of textiles for health care prod-uctsrdquo 4e Journal of the Textile Institute vol 106 no 7pp 706ndash717 2015
[36] I Gulccedilin ldquoAntioxidant antimicrobial antiulcer and analgesicactivities of nettle (Urtica dioica L)rdquo Journal of Ethno-pharmacology vol 90 no 2-3 pp 205ndash215 2004
[37] P Mantecca E Moschini P Bonfanti et al ldquoToxicity eval-uation of a new Zn-doped CuO nanocomposite with highlyeffective antibacterial propertiesrdquo Toxicological Sciencesvol 146 no 1 pp 16ndash30 2015
[38] V K Midha A Dakuri and V Midha ldquoStudies on theproperties of nonwoven surgical gownsrdquo Journal of IndustrialTextiles vol 43 no 2 pp 174ndash190 2013
[39] S W Ali S Rajendran and M Joshi ldquoSynthesis and char-acterization of chitosan and silver loaded chitosan nano-particles for bioactive polyesterrdquo Carbohydrate Polymersvol 83 no 2 pp 438ndash446 2011
[40] G M L Bearman A Rosato K Elam et al ldquoA crossover trialof antimicrobial scrubs to reduce methicillin-resistantStaphylococcus aureus burden on healthcare worker apparelrdquo
Infection Control amp Hospital Epidemiology vol 33 no 3pp 268ndash275 2012
[41] F Eser and A Onal ldquoDyeing of wool and cotton with extractof the nettle (Urtica dioica L) leavesrdquo Journal of NaturalFibers vol 12 no 3 pp 222ndash231 2015
[42] G Bag ldquoAssessment of total flavonoid content and antioxi-dant activity of methanolic rhizome extract of threeHedychium species of Manipur valleyrdquo International Journalof Pharmaceutical Sciences vol 30 no 1 pp 154ndash159 2015
[43] S ETHurovic ldquoChemical composition of stinging nettle leavesobtained by different analytical approachesrdquo Journal ofFunctional Food vol 32 pp 18ndash26 2017
[44] C S Ezeonu and C M Ejikeme ldquoQualitative and quantitativedetermination of phytochemical contents of indigenousNigerian softwoodsrdquo New Journal of Science vol 56 ArticleID 5601327 9 pages 2016
[45] H Y Fu S J Chen R F Chen W H Ding L L Kuo-Huangand R N Huang ldquoIdentification of oxalic acid and tartaricacid as major persistent pain-inducing toxins in the stinginghairs of the nettle Urtica thunbergianardquo Annals of Botanyvol 98 no 1 pp 57ndash65 2006
[46] Y Gao and R Cranston ldquoRecent advances in antimicrobialtreatments of textilesrdquo Textile Research Journal vol 78 no 1pp 60ndash72 2008
[47] S W Ali ldquoAntibacterial properties of aloe vera gel-finishedcotton fabricrdquo Cellulose vol 21 no 3 pp 2063ndash2072 2014
[48] M Gupta S +akur A Sharma and S Gupta ldquoQualitativeand quantitative analysis of phytochemicals and pharmaco-logical value of some dye yielding medicinal plantsrdquo OrientalJournal of Chemistry vol 29 no 2 pp 475ndash481 2013
10 Journal of Chemistry
[23] D Kut ldquoEffects of environmental conditions on the anti-bacterial activity of treated cotton knitsrdquo AATCC Reviewvol 5 no 3 2005
[24] N Afraz ldquoAntimicrobial finishes for textilesrdquo Including re-sults for Curr Trends Fashion Technology Textile Engineeringvol 5 p 4 2019
[25] A El-Shafei ldquoHerbal extract as an ecofriendly antibacterialfinishing of cotton fabricrdquo Egyptian Journal of Chemistryvol 61 no 2 pp 317ndash327 2018
[26] A Haji M Nasiriboroumand and S S Qavamnia ldquoCottondyeing and antibacterial finishing using agricultural waste byan eco-friendly process optimized by response surfacemethodologyrdquo Fibers and Polymers vol 19 no 11pp 2359ndash2364 2018
[27] A Reshma V B Priyadarisini and K Amutha ldquoSustainableantimicrobial finishing of fabrics using natural bioactiveagentsrdquo International Journal of Life Science vol 4 pp 10ndash202018
[28] W Ibrahim ldquoAloe vera leaf gel extract for antibacterial andsoftness properties of cottonrdquo Journal of Textile Science ampEngineering vol 7 no 301 p 2 2017
[29] P S Vankar R Shanker and S Wijayapala ldquoDyeing ofcotton wool and silk with extract of Allium cepardquo Pigment ampResin Technology vol 38 no 4 pp 242ndash247 2009
[30] G Singh ldquoFunctionalization of wool fabric using kapokflower and bio-mordantrdquo Sustainable Chemistry and Phar-macy vol 14 pp 2352ndash5541 2019
[31] K Gong Y Pan L J Rather et al ldquoNatural pigment duringflora leaf senescence and its application in dyeing and UVprotection finish of silk and woolmdasha case study of Cinna-momum camphorardquoDyes and Pigments vol 166 pp 114ndash1212019
[32] J Sheikh ldquoUltrasound assisted extraction of natural dyes andnatural mordants vis a vis dyeingrdquo Fibers and Polymersvol 17 no 5 pp 738ndash743 2016
[33] K Koszegi ldquoAntimicrobial Effects of the stinging nettle(Urtica dioica L)rdquo Analecta Technical Szegedinensia vol 11p 22 2017
[34] K Belay andM J C M R Sisay ldquoPhytochemical constituentsand physicochemical properties of medicinal plant (Moringaoleifera) around Bule Horardquo Chemistry and Materials Re-search vol 6 no 7 pp 61ndash72 2014
[35] K Murugesh Babu and K B Ravindra ldquoBioactive antimi-crobial agents for finishing of textiles for health care prod-uctsrdquo 4e Journal of the Textile Institute vol 106 no 7pp 706ndash717 2015
[36] I Gulccedilin ldquoAntioxidant antimicrobial antiulcer and analgesicactivities of nettle (Urtica dioica L)rdquo Journal of Ethno-pharmacology vol 90 no 2-3 pp 205ndash215 2004
[37] P Mantecca E Moschini P Bonfanti et al ldquoToxicity eval-uation of a new Zn-doped CuO nanocomposite with highlyeffective antibacterial propertiesrdquo Toxicological Sciencesvol 146 no 1 pp 16ndash30 2015
[38] V K Midha A Dakuri and V Midha ldquoStudies on theproperties of nonwoven surgical gownsrdquo Journal of IndustrialTextiles vol 43 no 2 pp 174ndash190 2013
[39] S W Ali S Rajendran and M Joshi ldquoSynthesis and char-acterization of chitosan and silver loaded chitosan nano-particles for bioactive polyesterrdquo Carbohydrate Polymersvol 83 no 2 pp 438ndash446 2011
[40] G M L Bearman A Rosato K Elam et al ldquoA crossover trialof antimicrobial scrubs to reduce methicillin-resistantStaphylococcus aureus burden on healthcare worker apparelrdquo
Infection Control amp Hospital Epidemiology vol 33 no 3pp 268ndash275 2012
[41] F Eser and A Onal ldquoDyeing of wool and cotton with extractof the nettle (Urtica dioica L) leavesrdquo Journal of NaturalFibers vol 12 no 3 pp 222ndash231 2015
[42] G Bag ldquoAssessment of total flavonoid content and antioxi-dant activity of methanolic rhizome extract of threeHedychium species of Manipur valleyrdquo International Journalof Pharmaceutical Sciences vol 30 no 1 pp 154ndash159 2015
[43] S ETHurovic ldquoChemical composition of stinging nettle leavesobtained by different analytical approachesrdquo Journal ofFunctional Food vol 32 pp 18ndash26 2017
[44] C S Ezeonu and C M Ejikeme ldquoQualitative and quantitativedetermination of phytochemical contents of indigenousNigerian softwoodsrdquo New Journal of Science vol 56 ArticleID 5601327 9 pages 2016
[45] H Y Fu S J Chen R F Chen W H Ding L L Kuo-Huangand R N Huang ldquoIdentification of oxalic acid and tartaricacid as major persistent pain-inducing toxins in the stinginghairs of the nettle Urtica thunbergianardquo Annals of Botanyvol 98 no 1 pp 57ndash65 2006
[46] Y Gao and R Cranston ldquoRecent advances in antimicrobialtreatments of textilesrdquo Textile Research Journal vol 78 no 1pp 60ndash72 2008
[47] S W Ali ldquoAntibacterial properties of aloe vera gel-finishedcotton fabricrdquo Cellulose vol 21 no 3 pp 2063ndash2072 2014
[48] M Gupta S +akur A Sharma and S Gupta ldquoQualitativeand quantitative analysis of phytochemicals and pharmaco-logical value of some dye yielding medicinal plantsrdquo OrientalJournal of Chemistry vol 29 no 2 pp 475ndash481 2013
