Optimization of yield for extraction of an essential oil from Cinnamon using

Microwave-assisted extraction

Prepared by : SatishKumar K. Movaliya

Enrollment no. : 150170730008

Guided by : Prof. Yogesh J. Morabiya

Vishwakarma Government Engineering College, Chandkheda

Ahmedabad-382424

31st May, 2017

Outlines

Research Objectives

Introduction

Microwave-assisted extraction

Research gap from literature survey

Experimental work

Design of Experiment (DOE)

Results

Conclusion

Future scope of work

References

To extract an essential oil from cinnamon by using novel technique –Microwave assisted extraction and Optimization of Microwaveextraction process parameter to obtain maximum yield of cinnamonoil.

To analyze the components which are present in essential oil by GC-

MS.

Comparison of novel techniques with hydrodistillation and find out thepredictive model by using ANN (Artificial neural network).

Research objectives

Properties of cinnamon oil

Scientific name : Cinnamomum verum, Cinnamomum cassia, Cinnamomumzeylanicum, Cinnamomum loureirii

Common name : Cinnamon, Cinnamomon, Ceylon cinnamon, Chinese cinnamon,Chinese cassia, Saigon cinnamon

Molecular formula : C9H8O

Molecular weight : 132.383 g/mol

IUPAC name : 2-methoxy-4-prop-2-enylphenol

Solubility : Soluble in 1-2.5 vols of 70% alcohol

Specific gravity : 1.020-1.030 at 20°C

Refractive index : 1.568-1.535 at 20°C

Introduction

Cinnamon

Introduction

Structure of cinnamon oil [67]Cinnamon sticks, powder and dried flowers [67]

Principle of microwave heating [65]

Microwave-assisted extraction

Microwave irradiation effect [65]

Microwave-assisted extraction

Before After

Representation of two heating modes : [31]

Microwave-assisted extraction

Important parameters in MAE

Selection of Solvent

Solvent-to-Feed Ratio (S/F)

Extraction time and cycle

Microwave power level

Extraction temperature

Stirring

Microwave-assisted extraction

Selection of solvents [65]

Microwave-assisted extraction

Solvent nameDielectric constant

Boiling point (°C) Viscosity (cP)

Acetone 20.7 56 0.30

Ethanol 24.3 78 0.69

Hexane 1.89 69 0.30

Methanol 32.6 65 0.54

2-Propanol 19.9 82 0.30

Water 78.3 100 0.89

Ethyl acetate 6.02 77 0.43

Research scholars or authors was used only HD andSCFE for extraction of cinnamon oil

Optimization method not applied

Not use water as a solvent

Research gap from literature survey

Plant material 1 kg Cinnamon bark collected

Pre-treatment procedure Washed into distilled water

Dried in open air for 1 day at temp. about 25-30°C

After drying Cinnamon crushed and grinded

After grinding Cinnamon powder was sieved by mechanical sieveshaker

Collect the Cinnamon powder which average particle size was less

than 100 μm

Experimental work

Experimental setup

Experimental work

RAGA’s Microwave system 20 liter capacityMaximum output power : 700 W Input power source : 250 V – 50 HzMicrowave frequency : 2450 MHz Cavity dimensions : 306 × 𝟐𝟏𝟏 × 320

mm

Microwave power level :140 W (20%) 210 W (30%)240 W (35%) 280 W (40%)350 W (50%) 420 W (60%)450 W (65%) 490 W (70%)560 W (80%) 700 W (100%)

Taguchi methodo Developed by Genichi taguchi

o It is a statistical method sometime called as Robust design method

o Employed this method for improve products or manufacturing processes

o Powerful and effective method to solve challenging quality problems

o Depending upon objectives three norms of mean square deviation

1. Nominal the better

2. Smaller the better

3. Larger the better

Design of Experiment (DOE)

Factors and their levels

Design of Experiment (DOE)

FactorsLevels

1 2 3 4

A Solid loading (gm) 20 25 30 35

B Solvent quantity (ml) 200 250 300 350

CMicrowave power level

(W)280 420 490 700

D Extraction time (min) 15 20 25 30

Design of Experiment (DOE)Run A B C D

Solid loading

(gm)

Solvent quantity

(ml)

Microwave power level

(W)

Extraction time (min)

1 1 1 1 1 20 200 280 15

2 1 2 2 2 20 250 420 20

3 1 3 3 3 20 300 490 25

4 1 4 4 4 20 350 700 30

5 2 1 2 3 25 200 420 25

6 2 2 1 4 25 250 280 30

7 2 3 4 1 25 300 700 15

8 2 4 3 2 25 350 490 20

9 3 1 3 4 30 200 490 30

10 3 2 4 3 30 250 700 25

11 3 3 1 2 30 300 280 20

12 3 4 2 1 30 350 420 15

13 4 1 4 2 35 200 700 20

14 4 2 3 1 35 250 490 15

15 4 3 2 4 35 300 420 30

16 4 4 1 3 35 350 280 25

ResultsExperimen

t no.Solid loading

(gm)

Solvent quantity

(ml)

Microwave power level

(W)

Extraction time (min)

Yield(%, w/w)

1 20 200 280 15 2.741

2 20 250 420 20 2.416

3 20 300 490 25 2.395

4 20 350 700 30 3.516

5 25 200 420 25 2.826

6 25 250 280 30 2.734

7 25 300 700 15 3.163

8 25 350 490 20 3.194

9 30 200 490 30 3.558

10 30 250 700 25 4.169

11 30 300 280 20 2.892

12 30 350 420 15 3.159

13 35 200 700 20 4.056

14 35 250 490 15 3.318

15 35 300 420 30 3.449

16 35 350 280 25 2.817

Parametric study

Results

Parametric study

Results

Parametric study

Results

Parametric study

Results

Fourier transform infrared spectroscopy (FTIR)

Results

Fourier transform infrared spectroscopy (FTIR)

Sample : Cinnamon powder before extraction

Results

Sr. no Wavenumber (cm-1) Functional group names

1 1004 Esters

2 1235 Ethers

3 1431 Nitro group

4 1555 Nitro group

5 1612 Alkenes, Amides, Amines

6 1654 Ketone, Esters, Alkenes

7 2924 Alkanes

8 3261 Alkynes, Phenols, Hydrogen O-H bonded

9 3732 Amines (Primary), Phenol

Fourier transform infrared spectroscopy (FTIR)

Results

Fourier transform infrared spectroscopy (FTIR)

Sample : Cinnamon powder after extraction

Results

Sr. no Wavenumber (cm-1) Functional group names

1 1026 Esters, Ethers

2 1089 Ethers

3 1613 Alkenes

4 3369 Carboxylic acids, Phenols

Gas chromatography–mass spectrometry (GC–MS)

Results

Gas chromatography–mass spectrometry (GC–MS)

Results

Probable Compound Retention time (min) Area (%)

𝛽-Methyl benzenepropanal 17.818 0.308

Cinnamaldehyde 21.644 89.324Copaene 24.869 0.807

Coumarin 27.611 0.675

(휀)-Cinnamyl acetate 28.002 0.273

𝛾 −Cadinene 29.177 0.325

𝛼 −Muurolene 30.236 1.569

𝛿 −Cadinene 31.236 2.950

𝛼 −Cadinene 31.653 2.225

Cadinadiene-1,4 35.373 0.404

𝛼 −Amorphene 35.933 0.761

𝛼 −Cadinol 36.094 0.383

ANOVA (Analysis of variance) Results

Results

ANOVA (Analysis of variance) Results

Results

ANN (Artificial neural network)

Results

Coefficient of Regression

for ANN in case of 7 hidden

neurons, FFBP algorithm and

log sigmoid transfer function

Results

R^2 = 99.527 %

Final model equation

Yield = 2.37 + [ 0.433 X1 – 0.00905 X2 – 0.00805 X3 – 0.3244 X4 – 000869 X1^2 +

0.00297 X4^2 + 0.000225 X1*X3 + 0.000463 X2*X4 + 0.000182 X3*X4

Where,

X1 : Solid loading (gm)

X2 : Solvent quantity (ml)

X3 : Microwave power level (W)

X4 : Extraction time (min)

Results

Optimum yield from predictive model by using ANN

Results

Solid Loading (gm) 35

Solvent quantity (ml) 250

Microwave power level (W) 700

Extraction time (min) 30

Predictive yield (%,w/w) 4.837

Actual yield (%,w/w) 4.814

Hydrodistillation method results

Results

Experiment no.

Solid loading(gm)

Solvent quantity (ml)

Extraction time (min)

Yield(%, w/w)

1

30 250

30 1.093

2 60 1.472

3 90 1.952

4 120 2.513

5 150 2.806

6 180 3.108

Gas chromatography–mass spectrometry (GC–MS)

Results

Probable Compound Retention time (min) Area (%)

Benzaldehyde 18.916 2.207

Borneol 20.584 1.529

Cinnamaldehyde 23.047 62.60Coumarin 26.087 1.298

𝛽-Cadinene 29.475 5.204

Trans-𝛼-Bengamotene 29.975 5.847

Camphor 30.236 3.742

𝛼-Humulene 31.380 2.950

Eugerol 32.065 4.603

Guaiacol 32.904 0.865

𝛼-Terpineol 34.237 3.507

Cubenol 34.564 5.602

Results

Collected oil

Comparison of MAE with HD

Results

Parameter MAE HDSolid loading (gm) 30 30

Solvent quantity (ml) 250 250

Microwave power level (W) 700 -

Extraction time (min) 30 180Maximum yield (%, w/w) 4.169 3.108

Microwave-assisted extraction is a rapid extraction technique forextraction of an essential oil.

In MAE method optimum conditions were obtained at solid loading 35

gm, solvent quantity 250 ml, microwave power level 700 W andextraction time 30 min.

Microwave power level is more significant parameter for rapidextraction.

MAE is more cost effective and environmental friendly technique.

Conclusion

To study the various properties of cinnamon oil

I. Anti-oxidant activity

II. Anti-microbial activity

III. Zone of inhibition

Future scope of work

1. Y. Li, D. Kong, and H. Wu, “Analysis and evaluation of essential oil components ofcinnamon barks using GC–MS and FTIR spectroscopy,” Industrial Crops andProducts, vol. 41, pp. 269–278, Jan. 2013.

2. R. Li, Y. Wang, Z.-T. Jiang, and S. Jiang, “Chemical Composition of the EssentialOils of Cinnamomum loureirii Nees. From China Obtained by Hydrodistillationand Microwave-assisted Hydrodistillation,” Journal of Essential Oil Research, vol.22, no. 2, pp. 129–131, Mar. 2010.

3. E. Schmidt et al., “Composition and antioxidant activities of the essential oil ofcinnamon (Cinnamomum zeylanicum Blume) leaves from Sri Lanka,” Journal ofEssential Oil Bearing Plants, vol. 9, no. 2, pp. 170–182, 2006.

4. N. Jeyaratnam, A. H. Nour, R. Kanthasamy, A. H. Nour, A. R. Yuvaraj, and J. O.Akindoyo, “Essential oil from Cinnamomum cassia bark through hydrodistillationand advanced microwave assisted hydrodistillation,” Industrial Crops and Products,vol. 92, pp. 57–66, Dec. 2016.

References

5. N. N. Kasim, S. N. A. S. Ismail, N. D. Masdar, F. Ab Hamid, and W. I. Nawawi,“Extraction and Potential of Cinnamon Essential Oil towards Repellency andInsecticidal Activity,” International Journal of Scientific and Research Publications,vol. 4, no. 7, 2014.

6. M. R. Thakker, J. K. Parikh, and M. A. Desai, “Microwave assisted extraction ofessential oil from the leaves of Palmarosa: Multi-response optimization andpredictive modelling,” Industrial Crops and Products, vol. 86, pp. 311–319, Aug.2016.

7. N. Jeyaratnam, A. H. Nour, and J. O. Akindoyo, “The potential of MicrowaveAssisted Hydrodistillation in extraction of essential oil from cinnamomum cassia(cinnamon),” 2006.

References

Paper publication

Satish Kumar M, “Optimization of Yield for Extraction of anEssential Oil from Cinnamon using Microwave-AssistedExtraction”, Journal of Chromatography & Separationtechniques, 2017. ISSN:2157-7064.

Paper publication

Questions ?

Thank you.