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PRODUCTION OF HAIR GROWTH HERBAL SHAMPOO BY USING ALEURITESMOLUCCANA SEEDS EXTRACT
NUR ANEESA ABDUL HALIM
Malaysian Institute of Chemical and Bioengineering TechnologyUniversiti Kuala Lumpur
SEPTEMBER 2015
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PRODUCTION OF HAIR GROWTH HERBAL SHAMPOO BY USING ALEURITESMOLUCCANA SEEDS EXTRACT
NUR ANEESA ABDUL HALIM
55101313060
A thesis submitted in fulfillment of theRequirements for the award of the
Diploma of Chemical Engineering Technology (Process)
Malaysia Institute of Chemical and Bioengineering TechnologyUniversiti Kuala Lumpur
SEPTEMBER 2015
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ABSTRACT
Hair loss is common condition and affects most people at some time in their
lives. Hair loss is because of factors such as predetermined genetic factors and the
overall aging process. It often presents suddenly with loss of the hair at the follicle
and affects most people of all range of age and gender. However there are
treatments that can regrowth the hair by using shampoo. Shampoo is a formulation
that used for washing of hair and scalp, packed in a form convenient for use. Each of
these ingredients have special role in shampoo’s formulation. Therefore, this study is
conducted to produce a hair growth herbal shampoo by using herb extracts which is
Aleurites Moluccana seeds extracts that traditionally act as the hair growth promoter.
The main objective of this research is to study the process of extraction of Aleurites
Moluccana Oil by using Ultrasonic-Assisted Extraction, to study the production of hair
growth herbal shampoo by using formulation gathered and to evaluate and compare
the formulated hair growth herbal shampoo by using Aleurites Moluccana Seeds
Extracts with the marketed shampoo. Therefore, the process of extraction of
Aleurites Moluccana oil by using Ultrasonic-Assisted Extraction and production of
hair growth herbal shampoo by using formulation gathered successfully conducted.
Besides, most of shampoo evaluation’s criteria of formulated hair growth herbal
shampoo are in the range with the marketed shampoo. Hence, the formulated hair
growth herbal shampoo is preferable to be produced.
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ABSTRAK
Keguguran rambut ialah satu situasi yang biasa dan memberi kesan kepada
kebanyakan orang pada suatu masa dalam hidup mereka. Keguguran rambut adalah
kerana faktor-faktor seperti faktor genetik telah ditetapkan dan proses penuaan
secara keseluruhan. Keguguran rambut sering terjadi secara tiba-tiba dengan
kehilangan rambut di folikel serta memberi kesan kepada kebanyakan manusia
pelbagai umur dan jantina. Walau bagaimanapun, terdapat rawatan yang boleh
pertumbuhan semula rambut dengan penggunaan produk syampu. Syampu adalah
satu formula yang digunakan untuk mencuci rambut dan kulit kepala, diproduk dalam
bentuk yang mudah untuk digunakan. Setiap satu daripada bahan-bahan ini
mempunyai peranan yang istimewa dalam pembuatan syampu ini. Oleh itu, kajian ini
dijalankan untuk menghasilkan syampu herba yang meningkatkan pertumbuhan
rambut dengan menggunakan ekstrak herba Aleurites Moluccana yang biasanya
bertindak meningkatkan pertumbuhan rambut. Objektif utama kajian ini adalah untuk
mengkaji proses pengekstrakan Aleurites Moluccana dengan menggunakan cara
ultrasonic. Selain itu, ia untuk mengkaji pembuatan syampu herba untuk
pertumbuhan rambut dengan menggunakan rumusan yang sedia ada dan untuk
menilai serta membandingkan syampu tersebut dengan syampu yang dipasarkan.
Oleh itu, proses pengekstrakan Aleurites Moluccana dan pengeluaran pertumbuhan
rambut syampu herba dengan menggunakan rumusan yang disediakan berjaya
dijalankan. Selain itu, sebahagian besar daripada kriteria penilaian syampu ini adalah
di dalam julat yang sama dengan syampu yang dipasarkan. Oleh itu, syampu herba
yang diprodukkan adalah selamat untuk digunakan dan dipasarkan.
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APPROVAL PAGE
I have Supervised and examined this report and verify that it meets the programmedand University’ requirements for the Diploma in Chemical Engineering Technology
(Process).
Date: Signature:
Supervisor’s Name: Marmy
Roshaidah binti Mohd Salleh
Official Stamp
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DECLARATION
I declare that this thesis entitled Production of Hair Growth Herbal Shampoo by using
Aleurites Moluccana Seeds Extract is the results of my own research except as cited
in the references. The thesis has not been accepted for any diploma and is not
concurrently submitted in submission of any other diploma.
Signature :
Name : Nur Aneesa binti Abdul Halim
Date : 19 December 2015
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To my family and friends
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ACKNOWLEDGEMENT
First of all, I am grateful to Allah s.w.t for his blessings and giving me the
strength and effort to accomplish this final project successfully as schedule.
I wish to express my sincere appreciation to my supervisor, Madam Marmy
Roshaidah Salleh for encouragement, valuable guidance and advice. She inspired
me greatly to work in this project. Besides, I am thankful to all process and technical
foundation department and technicians for their guidance, advices and motivation.
Without their support and interest, the thesis would not have been the same as
presented here.
I would like to thank my fellow colleagues; Nor Razila, Nursyamimi, Nur
Hidayah and others who help me and give support to finish this project. Their views
and tips are useful indeed .Lastly and most important, I wish thank to my beloved
parents, Mr. Abdul Halim and Mrs. Azlina and my beloved family. They continuously
supported me, taught me and love me.
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TABLE OF CONTENTS
TITLE PAGE
TITLE PAGE ii
ABSTRACT iii
ABSTRAK iv
APPROVAL v
DECLARATION vi
DEDICATION vii
ACKNOWLEDGEMENT viii
TABLE OF CONTENT ix
LIST OF TABLES xii
LIST OF FIGURES xiii
LIST OF APPENDICES xvi
1. CHAPTER 1 INTRODUCTION
1.1 Background study 1
1.2 Problem statement 2
1.3 Objectives 3
1.4 Scope of study 4
1.5 Thesis Layout 5
2. CHAPTER 2 LITERATURE REVIEW
2.1. An overview 6
2.2. Hair Loss (Alopecia) 6
2.2.1. Type of Alopecia 8
2.2.2. Cause of Alopecia 9
2.2.3. Treatment of Alopecia 9
2.3. Shampoo 10
2.3.1. Basic Ingredient of Shampoo 11
2.3.2. Type of shampoo 132.3.3. Herbal Shampoo 14
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2.3.4. Evaluation and Quality Control of Shampoo 17
2.4. Aleurites Moluccana 18
2.4.1. Scientific Classification 19
2.4.2. Origin and Distribution of Aleurites Moluccana 20
2.4.3. Description of Aleurites Moluccana 20
2.4.4. Application of Aleurites Moluccana 22
2.4.5. Aleurites Moluccana Oil as Remedy 24
2.5. Extraction Method 25
2.5.1. Ultrasonic-Assisted Extraction 26
2.6. Solvent 27
2.6.1. Acetone 28
3. CHAPTER 3 METHODOLOGY
3.1. An overview 29
3.2. Methodology Overview 29
3.3. Materials 30
3.4. Equipment 30
3.5. Procedures 31
3.5.1. Preparation of Aleurites Moluccana Seeds 32
3.5.2. Extraction of Aleurites Moluccana Seeds 33
3.5.3. Filtration Process 34
3.5.4. Rotary Evaporating Process 35
3.5.5. Formulation of Hair Growth Herbal Shampoo 36
3.5.6. Shampoo Evaluation Process 38
3.5.6.1. Physical appearance or visual 38
inspection
3.5.6.2. Determination of pH value 38
3.5.6.3. Percentage of solid content 39
3.5.6.4. Wetting time 39
3.5.6.5. Rheological property 39
3.5.6.6. Foam volume and stability 40
3.5.6.7. Eye irritation test 40
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4. CHAPTER 4: RESULTS AND DISCUSSIONS
4.1. An overview 41
4.2. Process of extraction of Aleurites Moluccana 42
4.2.1. Sample preparation 42
4.2.2. Extraction of Aleurites Moluccana Seeds 43
4.2.3. Filtration and Rotary Evaporating Process 44
4.3. Production of Hair Growth Hair Shampoo 45
4.3.1. Formulation of Hair Growth Herbal Shampoo 46
4.3.2. Process of Production of Hair Growth Herbal 47
Shampoo
4.3.3. Hair Growth Herbal Shampoo by using 48
Aleurites Moluccana Extracts
4.4. Shampoo Evaluation Process 49
4.4.1. Physical appearance and visual inspection 50
4.4.2. Determination of pH value 51
4.4.3. Percentage of solid content 52
4.4.4. Wetting time 53
4.4.5. Rheological property 54
4.4.6. Foam volume and stability 56
4.4.7. Eye irritation test 57
5. CHAPTER 5 CONCLUSION AND RECOMMENDATION
5.1. Conclusion 59
5.2. Recommendations 60
5.2.1. Determination of Active Ingredient in Aleurites 60
Moluccana Seeds Extracts
5.2.2. Observation of Hair Growth of Specimen 60
by using Aleurites Moluccana Seeds Extracts
5.2.3. Optimization of Hair Growth of Specimen by 60
using Hair Growth Herbal Shampoo
REFERENCES 61
APPENDICES 65
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LIST OF TABLES
TABLE NO TITLE PAGE NO
2.1 Type of Alopecia and its descriptions on characteristic of
different alopecia
8
2.2 The Common Herbs used which benefits the hair with its
functions
15
2.3 The Scientific Classification of Aleurites Moluccana 19
2.4: The Applications of Aleurites Moluccana 22
3.1 The formulation of herbal shampoo 36
4.1 The formulation of herbal shampoo 46
4.2 The results for Shampoo Evaluation Process 49
4.3 The results for Rheological properties 54
4.4 Volume of foam produced by shampoo 56
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LIST OF FIGURE
FIGURE NO TITLE PAGE
2.1 The process of hair loss on hair scalp. 7
2.2 Example of shampoo which is Suave Shampoo, Pantene
Shampoo and Herbal Essences Shampoo.
10
2.3: Example of Herbal Shampoo 14
2.4 Fruit branch of Aleurites Moluccana tree 18
2.5: The parts of Aleurites Moluccana fruit. 21
3.1 The overview of methodology of Production of Hair
Growth Herbal Shampoo by using Aleurites Moluccana
Seeds Extracts
29
3.2 The raw material used for formulation of shampoo 30
3.3 Ultrasonic Bath from brand D-78224 Singan/Htw Elma 31
3.4 Rotary Evaporator 31
3.5 Removal of moisture content in Aleurites Moluccana
Seeds
32
3.6 The blended Aleurites Moluccana Seeds 32
3.7 The mixed Aleurites Moluccana seeds and solvent 33
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solution
3.8 The mixed Aleurites Moluccana seeds and solvent
solution is immersed in ultrasonic bath.
33
3.9 The filtration process of Aleurites Moluccana seeds and
remaining mixed solvent and oil extracted
34
3.10 The overview of formulation of herbal shampoo 35
3.11 The mixing of the ingredients of the formulations 37
3.12 The determination of pH value of shampoo by using pH
meter
38
3.13 The solid content test on the shampoo 39
4.1 Aleurites Moluccana Seeds after undergo the sample
preparation
42
4.2 The sample of oil extracted 45
4.3 The weight of oil extracted after three times repeat the
procedure of extraction method.
45
4.4 Final product of hair growth herbal shampoo by using
Aleurites Moluccana seed extracts
48
4.5 Physical Appearance of shampoo 50
4.6 The pH value against the type of shampoo 51
4.7 The Percentage of solid content against Type of shampoo 52
4.8 Wetting Time against Type of Shampoo 53
4.9 Viscosity (mPa.s) against Spindle speed (rpm) 55
4.10 Volume of foam (ml) against time intervals (minute) 56
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4.11 Eye of lab rat specimen before treatment with formulated
hair growth herbal shampoo
57
4.12 Eye of lab rat specimen after treatment with formulated
hair growth herbal shampoo
58
4.13 Eye of lab rat specimen before treatment with marketed
shampoo
58
4.14 Eye of lab rat specimen before treatment with marketedshampoo
58
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LIST OF APPENDICES
APPENDIX TITLE PAGE
A Viscosity Calculation 81
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CHAPTER 1
INTRODUCTION
1.1. Background Study
Hair loss is common condition and affects most people at some time in their
lives. Most hair loss is a result of predetermined genetic factors and the overall aging
process. Many men and women notice mild physiologic thinning of hair starting in
their 30’s and 40 ‘s. Illness, emotional trauma, protein deprivation and hormonal
changes may cause a reversible hair loss. Therefore, shampoos are invented as a
medicine to cure the hair loss and cultivate the hair growth of the consumers.
Shampoo is a formulation that used for washing of hair and scalp, packed in a
form convenient for use. The primary function is of cleansing the hair of accumulated
sebum, scalp debris and residues of hair-grooming preparation. It has manyproperties in addition in their detergency such as hair growth, conditioning and hair
shining. They are expected to be non-irritating to skin and mucous membranes
(Hilda, 1996). There are many different varieties of ingredients to make a proper
shampoo. Each of these ingredients have special role in shampoo’s formulation.
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The major ingredient used in making a shampoo are detergents, conditioning
and active ingredients for hair manageability, additives that modify the surfactant
effect, stabilize the product which is preservatives and anti-oxidants and increase its
appeal by inserting fragrances, dyes, essence and anti-UV light protector.
Discussions about hair product are on demand nowadays. Hair tonic by using
herbs extracts are used such as Fenugreek extracts and Nigella Sativa. This is
because people are using herbs for cleaning, beautifying and managing hair since
the ancient era. As the time has passed, synthetics agents have taken a large share
but today people are getting aware of the harmful effects on hairs, skin and eyes.
Hence, the community are attracted to herbal product which has negligible side effect
and has higher efficiency than marketed shampoos. This is because the present
invention of herbal shampoo will provide a method for hair growth and to overcome
the hair loss problem. Besides it will support eco-friendly products and save the
environment. Therefore, this study is conducted to produce a hair growth herbal
shampoo by using a different herb extracts which is Aleurites Moluccana (A.
Moluccana) seeds extracts that traditionally act as the hair growth promoter.
A.Moluccana is another member of Euphorbiaceous family. It is generically
known as the candle nut tree and Hawaiian tree. It thrives in wet or dry subtropical
and tropical forest zones. A. Moluccana tree produces spherical fruits, with a thickand hard nut shell making up to 64-68% of fruit, and the nut shell is difficult from its
oil-rich kernel. Oil production of A. Moluccana varies from 15% to 20% of nut weight.
The oil is rich in polyunsaturated oils; linolenic, oleic and various linoleic acids.
(Kizazohi, Sangwan.R.S, 2011).
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1.2. Problem Statements
Hair loss is common problem affecting both men and women from all range of age. It
is one of prevalent issues in the 21st century. All mankind can suffer hair loss which is
resulted of one factor or combination of factors including genetic factors, hormonalfactors, surgery, trauma and stress. Illian Bandaranayake, Paradi Mirmirani stated
that “Hair loss often have significant negative impacts to self -esteem and body
image”. Hence, remedies for hair growth have been proposed.
A remedy which is shampoo products has become a popular form of
healthcare. It needs to be tested for the efficiency using conventional methodology
and several specific extracts have been demonstrated to be efficacious for specific
conditions. Nevertheless the public is often misleading to believe that all hair growth
shampoo managed to overcome hair loss problem by increases the hair growth but it
may create other new problems from the usage of synthetic hair growth promoter.
Thus extracts of herbal ingredient is used instead of synthetic ingredient. To study
this problem, production of Hair Growth Herbal Shampoo by using extracts of
Candlenut or the scientific name Aleurites Moluccana (A. Moluccana) have been
proposed.
Frequently, there are several marketed products containing A. Moluccana oil.
According to Adida Muhammad (2014), A. Moluccana oil contains substantial
amounts of anti-aging component known as omega-3 fatty acids that helps to
strengthen and restore radiance to the hair. Meanwhile, Noviansyah and Sidharta
(2009) stated that A. Moluccana oil is always used as an ingredient for traditional
medicine to prevent hair loss and enhance hair growth.
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1.3. Objectives
The objectives of the study can be outlined as follows:
1. To extract Aleurites Moluccana Oil from Aleurites Moluccana Seeds.
2. To produce Hair Growth Herbal Shampoo by using extracts of Aleurites
Moluccana Seeds.
3. To study the shampoo evaluation process of Hair Growth Herbal Shampoo by
using extracts of Aleurites Moluccana Seeds and compare with marketed
shampoo.
1.4. Scope of Study
Three scopes are focused to produce hair growth herbal shampoo by using Aleurites
Moluccana Seeds Extracts.
1. To focus on process of extraction of Aleurites Moluccana seeds using
Ultrasonic-Assisted Method.
2. Development of production of hair growth herbal shampoo from formulation.
3. Analysis of shampoo evaluation process of formulated hair growth herbal
shampoo compared to marketed shampoo which is Follow Me shampoo.
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1.5. Thesis Layout
The thesis layouts for final year project are as below:
i. Chapter 1 is the background study of hair loss, shampoos and AleuritesMoluccana. The problem statement and the objective of the research also
stated in chapter 1.
ii. Chapter 2 is about the literature review that is related to the research that
is being done such as the hair loss disease including treatment of hair
loss disease, shampoo background study, method use in the experiment,
solvent, extraction method and Aleurites Moluccana species.
iii. Chapter 3 is the methodology of sample preparation throughout this
research such as preparation of material extracts, procedure for the
experiment, the formulation of hair growth hair shampoo and quality
testing for formulated product.
i. Chapter 4 is the discussion regarding the shampoo evaluation process of
formulated hair growth herbal shampoo by using Aleurites Moluccana
Seeds Extracts and compare with marketed shampoo.
iv. Chapter 5 is the conclusion for the experiment and the recommendation
that can be done in the future to improve the research of production of
hair growth herbal shampoo by using Aleurites Moluccana Seeds
Extracts.
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CHAPTER 2
LITERATURE REVIEW
2.1. An overview
This chapter provides a brief review on production of hair growth herbal
shampoo followed by specific information on the important data collected during this
study. The process used was also briefly reviewed and other information relevant to
this study. The aim of this chapter was to obtain information that would provide the
context within this study which could be undertaken more comprehensively.
2.2. Hair Loss (Alopecia)
Alopecia which is a general medical term for hair loss is a common patientcondition and affects most people in their lives. Alopecia is characterized by partial or
complete loss of hair that leaves the skin bald. Hereditary disorders, aging, hormonal
imbalance, internal and infectious diseases, intoxication and trauma affect hair
losses. Usually, hair loss is most noticeable on the scalp but it can occur anywhere
on the body where the hair grows. “The relevant hair loss etiology includes male
pattern hair loss (MPHL), female pattern hair loss (FPHL), telogen effluvium (hair loss
due to a traumatic event), and senescent alopecia (hair loss due to aging). Figure 2.1
shows the process of hair loss on hair scalp from time to time.
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Figure 2.1: The process of hair loss on hair scalp
Hair loss is a cause of great distress for both men and women, producing
significant psychosocial discomfort, and studies reveal that balding men are looked
upon more negatively than non-balding men. Few physical attributes are more
associated with aging than hair loss, and unfortunately along with the lost hair it may
be presumed that virility, strength, and attractiveness are lost as well.” (Robert S.
Haber, 2014)Hair loss may cause great distress for both men and women, producing
significant psychosocial discomfort, and studies reveal that balding men are looked
upon more negatively than non-balding men. Few physical attributes are more
associated with aging than hair loss, and unfortunately along with the lost hair it may
be presumed that virility, strength, and attractiveness are lost as well. (Robert S.
Haber, 2014)
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2.2.1. Type of Alopecia
According to Robert S. Haber, there are four different type of Alopecia which
is Androgenic Alopecia, Alopecia Areata, Telogen effluvium and Sensescent
Alopecia. Table 2.1 shows the type of Alopecia and its descriptions on characteristicof different alopecia.
Table 2.1: Type of Alopecia and its descriptions on characteristic of different alopecia
(Robert S. Haber, 2014)
Alopecia Descriptions
Androge-
nic
alopecia
Androgenetic alopecia occurs in both males and females. Well-
evidenced therapies are oral finasteride and topical minoxidil for male
androgenetic alopecia and topical minoxidil for female androgenetic
alopecia. Best way to surgically obtain natural appearance is
transplantation of follicular units from non-bald occipital skin to bald
scalp skin.
Alopecia
areata.
Alopecia areata is a chronic inflammatory disease characterized by non-
scarring hair loss on the scalp or any hair bearing skin and sometimes
the nail deformity. A number of treatments can induce hair growth in
alopecia areata, but they do not cure the condition.
Telogen
effluvium.
In this condition, diffuse hair loss occurs, often proceeded by a
significant stress such as fever, childbirth, illness, psychological stress,
or other disease state. In most cases, full hair regrowth can be seen,
but a chronic form of the condition exists, and a careful clinical and
laboratory investigation is warranted. Prompt identification of treatable
conditions including endocrine abnormalities, anaemia, nutritional
deficits, and other systemic illnesses will improve the prognosis.
Sensesc-
ent
Alopecia
Also termed senile alopecia, this is a relatively new hair loss category
that recognizes the inevitable effects of the aging process on the hair
follicle independent of any other factors. In this condition, both men and
women experience slowly progressive hair loss in a non-patterned
distribution, generally after the seventh decade. There is no scalp
inflammation, and the hairs are simply reduced in number and size. It
may be that depletion of the stem cell reservoir required for hair follicle
regeneration produces this condition.
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2.2.2. Cause of Alopecia
Alopecia is generally caused by inactivation or destruction of the hair follicles
preceded by a gradual shrinkage and miniaturizing. Even nowadays, it has been
believed that hair follicles form only during embryonic development and a fixednumber of hair follicles of each individual are born with. In 1998 Gat et al. reported
findings on de novo hair follicle morphogenesis in adult skin and this has created
possible strategies for the regeneration and reactivation of miniaturized hair follicles.
2.2.3. Treatment of Alopecia
Recently, there are current treatments to promote hair regrowth in patients. It
includes oral finasteride, topical minoxidil solutions, low-level laser light, shampoos
and hair transplant. There is varied treatment efficacy and all treatments except
shampoos are generally recommended only for patients whose medication has failed
(Varothai and Bergfeld, 2014).
Minoxidil is a potent vasodilator, acting on potassium channels (Messenger
and Rundegren, 2004). However, vasodilation appears to have no effect on hair
growth and its mechanism for treating alopecia is not clear (Shorter et al., 2008).
Minoxidil improves miniaturisation in most scalp regions, but only promotes hair
growth on the vertex scalp (Olsen et al., 2007). The adverse effects of minoxidil are
contact dermatitis, facial hypertrichosis and a temporary increase in hair shedding
(Varothai and Bergfeld, 2014). Telogen effluvium has been reported after treatment
has stopped (Banka et al, 2013).
However, formulated shampoo has been found by the researcher as a way to
treat alopecia which is by using formulated basic shampoo ingredient with extracted
herbs. It is because herbs can act as hair growth promoter and does not have any
side effects (Jansen, 2010) Natural remedies have been used for centuries fortreating alopecia (Chandra Shekar BR, 2015). In traditional Indian system of
medicine many plants and herbal formulations are reported for hair growth promotion
as well as improvement of quality of hairs (Thakur R, 2015)
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2.3. Shampoo
One of common problem solver for hair treatment is Shampooing. Shampoos
are kind of formulation that are used for hair and body washing or therapeutic
purposes. However, shampoos have primarily been products aimed at cleansing thehair and scalp. Shampoos are expected to be much more than mere cleansing
agents. It has many properties in addition of their detergency, such as conditioning
and hair shining. They are expected to be non-irritating to skin and mucous
membranes (Yentzer, 2009). The main function of shampoo is cleansing of the hair
necessitated due to accumulated sebum, dust, scalp debris etc. Various shampoo
formulations are associated with hair quality, hair care and specific hair problems
such as treatment of oily hairs, dandruff and for androgenic alopecia. There are
different types of shampoo which is in form of liquid, creamy or gel shampoos. Figure
2.2 shows an example of shampoo which is Suave Shampoo, Pantene Shampoo and
Herbal Essences Shampoo.
Figure 2.2: Example of shampoo which is Suave Shampoo, Pantene Shampoo and
Herbal Essences Shampoo.
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2.3.1. Basic Ingredient of Shampoo
A shampoo consists of different types of ingredients in order to produce a
proper shampoo. Each of these ingredients has its own special role in shampoo’s
formulation. The major ingredients used in making a shampoo are detergents(surfactants), conditioning and active ingredients for hair manageability, additives that
modify the surfactant effect which is viscosity control agents, foam stabilizers and
viscosity modifiers. Besides that, to stabilize the product it will consist of
preservatives and anti-oxidants and to increase its appeal, the shampoo will needed
fragrances, essence, anti-UV light protector, dyes and ingredients for consistency
and a pearlescent appearance.
Surfactants are the main ingredients that are compulsory to be added in the
shampoo. It is briefly defined and functions as a material that can greatly reduce the
surface tension of water when used in very low concentrations. Some compounds
are amphiphilic or amphipathic which is they have one part that has an affinity for
nonpolar media and one part that has an affinity for polar media. These molecules
form oriented monolayers at interfaces and showed the surface activity. In some
usage surfactants are defined as molecules capable of associating to form micelles.
These compounds are termed surfactants, amphiphiles, surface-active agents,
tensides or paraffin chain salts. The most commonly used term, surfactant, wasoriginally registered as a trademark for selected surface-active products. . There are
different types of surfactants which are anionic surfactants, non-ionic surfactants and
cationic surfactants. (Salager, 2012)
Anionic surfactants are dissociated in water in an amphiphilic anion, and a
cation, which is in general an alkaline metal (Na+, K+) or a quaternary ammonium.
They are the most commonly used surfactants. They include alkyl benzene
sulfonates (detergents), (fatty acid) soaps, lauryl sulfate (foaming agent), di-alkyl
sulfosuccinate (wetting agent), lignosulfonates (dispersants) etc. Meanwhile, non-
ionic surfactants do not ionize in aqueous solution, because their hydrophilic group is
of a non-dissociable type, such as alcohol, phenol, ether, ester, or amide. A large
proportion of these non-ionic surfactants are made hydrophilic by the presence of a
polyethylene glycol chain, obtained by the poly condensation of ethylene oxide. They
are called polyethoxylated non-ionic. Other than that, the Cationic Surfactants are
dissociated in water into an amphiphilic cation and an anion, which is most often of
the halogen type. A very large proportion of this class corresponds to nitrogen
compounds such as fatty amine salts and quaternary ammoniums, with one or
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several long chain of the alkyl type, often coming from natural fatty acids. These
surfactants are in general more expensive than anionic, because of the high pressure
hydrogenation reaction to be carried out during their synthesis. Lastly, Zwitterionic
Surfactants is a type of surfactant when a single surfactant molecule exhibit both
anionic and cationic dissociations. This is the case of synthetic products like betaines
or natural substances such as phospholipids. Some Zwitterionic surfactants are
insensitive to pH, whereas others are cationic at low pH and anionic at high pH, with
Zwitterionic behavior at intermediate pH. Zwitterionic surfactant is quite expensive,
and their use is limited to very special applications such as cosmetics where their
high biological compatibility and low toxicity is of primary importance. (Salager, 2012)
Some of additives are not compulsory to be added to while many of them
have to be added in a shampoo formulation in order to increase its stability and
safety. (Trüeb, 2007) One of example of the additives is conditioning agent. They
have been attractive components. Surfactants are specific conditioners however
there are many other materials used as conditioners. As an example of conditioning
agent are paraffin and lanolin. There are also many other materials that serves as
conditioners which is peptides, egg derivatives and synthetic resin. These materials
were added in shampoo formulation as hair conditioner and hair shining agents.
Other polymers used in the formulation of shampoos that are capable of drawing
crisp hair could be water soluble phosphate salts and amino ethyl ester poly acrylic
acid. The resin is used in the formulation of shampoos containing surfactants.
(Rosen, 1989)
Viscosity control agents, foam stabilizers and viscosity modifiers are an
important part of the marketing plan for a personal care product like shampoo. Most
consumers buy products because of its appearance, smell, color and packaging. A
nice thick viscosity looks appealing and it also provides the perception of being
“concentrated” and more value for the money as compared to a thin, runny product.Examples of excellent viscosity builder are sodium chloride, betaines and amides. A
formulator should avoid going over the maxima for the salt-viscosity curve. After the
maxima, a further increase of salt will decrease the formula’s viscosity, in some
cases quite sharply. Polymers both natural and synthetic, can also serve as viscosity
builders.
Almost all shampoo formulas include minor ingredients to stabilize the
product it will consist of preservatives and anti-oxidants and to increase its appeal
and the shampoo will needed fragrances, essence, anti-UV light protector, dyes and
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ingredients for consistency and a pearlescent appearance. Common preservatives
for shampoo formula include methylchloroisothiazolinone, methylisothiazolinone,
DMDM hydantoin and quaternium-15. There are preservative tests to be run as it is
to ensure that the product has proper protection against any microorganism attack.
There is a wide variety of perfume compounds available on the market. A perfume
must be compatible and soluble with the shampoo formula. Some perfumes may
need additional solubilizer like polysorbate added to the formula to achieve proper
solubility.
2.3.2. Type of shampoo
Currently, there are several type of shampoo existed such as liquid shampoo,
solid shampoo and specialized shampoo. Solid shampoo is a shampoo in form solid
such as bars that use as their surfactants formulated as solids. Solid forms have the
benefits of being spill-proof and it is easy to apply and work the soaped hair into a
low lather.
Within recent years, shampoos of the liquid creamy or milky type have been
developed and possess a number of advantages as they have a pleasing creamy-like
appearance. That appearance is relatively good emulsifiers, lather profusely, etc. Ithas been attempted recently to prepare shampoos having the desirable features of
both the liquid and paste types of shampoo whereby there may be unitarily obtained
a creamy opaque like appearance of such consistency that the material flows from a
suitable container at normal temperature. There are still a number of problems which
are of general concern however with regard to liquid cream shampoos. A primary
consideration has been the general instability of these liquid types, such that at
temperatures of up to about 110 F., phase separation occurs and translucent results.
It has been said that such types of shampoos are better known for their perversitythan for their stability (Henkin Hyman, 1953).
Other than that, specialized shampoo is one type of shampoo. Examples of
specialized shampoos are such as Conditioning shampoo, Antidandruff shampoo,
Baby shampoo, two in one shampoo etc. Two in one shampoo is a shampoo which
cleansing formulations have gradually changed from a stage of pure cleansing of the
hair or skin to a 2-in-1 type or to multifunctional purposes (Schueller R, 2003). Other
examples of the benefits of multifunctional purposes include conditioning, smoothing
and lather creaminess (Sander R, 2000). Conditioners shampoos are liquids,
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creams, pastes, or gels that mimic sebum in making the hair manageable, glossy,
and soft. The role of conditioners goes beyond maintaining the appearance of
healthy hair. Conditioners also attempt to recondition hair that has been damaged by
chemical or mechanical trauma (Brown AC, 1972).
2.3.3. Herbal Shampoo
Recently, the whole world is turn towards the use of herbal products and to
adopt more natural way of life. Consumers prefer herbal medicine and natural curing
practices for a healthy life. The usage of herbal cosmetics and demand for herbal
cosmetics increases. This is due to excessive uses of synthetic based products,
chemical dyes and derivatives products that cause several health hazards with side
effects that lead to numerous diseases. The eco-system is affected by the
environmental pollution caused by those synthetics products (Kapoor VP, 1999).
The search for hair shampoo results into few treatments of synthetic origin.
However there are few side effects of synthetic shampoos. Thus, herbal ingredients
in the formulation are viable alternative to synthetic shampoo. Natural remedies have
been used for centuries for treating alopecia (Chandra Shekar BR, 2015). In
traditional Indian system of medicine many plants and herbal formulations arereported for hair growth promotion as well as improvement of quality of hairs (Thakur
R, 2015). Based on figure 2.3, it is an example of 100 hair growth products are
available in the markets which are prepared by combination of one or more herbal
ingredients (Thakur R, 2015). Although herbal ingredients are currently widely
accepted by the patient, the scientific review among dermatologists is limited.
Figure 2.3: Example of Herbal Shampoo
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Recently, various plant extract have been patented for use in hair growth or
hair tonic products, and for prevention of alopecia (Chandra Shekar BR, Nagarajappa
R, Suma S, Thakur R, 2015). Suriya Prakash et al. formulated herbal shampoo for its
anti-microbial and anti-lice activity. The natural ingredients used are neem leaf,
thulasi leaf and gooseberry fruit. The prepared formulations were evaluated for its
physicochemical properties, antimicrobial and anti-lice activity, which was compared
with the marketed products. Table 2.2 shows the common herbs used and its
function which benefits for healthy hair.
Table 2.2: The Common Herbs used which benefits the hair with its functions.
(Neeharika Rallapally et.al, 2013)
Botanical Name Common name Function
Sapindus
mukorrosi
Soapnuts An excellent hair tonic, long known for its
benefits for healthy hair. The natural
saponin not only cleanses hair, they add
body and sheen and make hair feel
thicker, silky and smooth.
Hibiscus sabdariffa Hibiscus One of the most common flowering trees
of India In hair care it is used to lessen
gray hair and promote hair growth. Thewoman of India used the Hibiscus flower
to adorn her hair, and used its extracts as
a treatment to thicken hair. The flowers
and leaves contain many properties that
benefit hair and scalp.
Acacia concinna Shikakai It has a naturally mild pH, as a natural hair
conditioner, Shikakai is said to promote
hair growth, strengthen hair roots and
clear dandruff.
Prunus dulcis Almond Oil It has moisturizing, nourishing properties
and is easily absorbed. In hair care, sweet
almond oil helps condition, nourish, and
soften hair.
Cera alba Beeswax In hair care Beeswax adds moisture,
hydration, and softness to hair and can
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add shine and glossiness to dull hair.
Phyllanthus emblica, Amla An excellent hair conditioning herb that
provides nourishment that penetrates the
scalp and strengthens hair at its root to
promote stronger, healthier new growth
and help with hair loss by normalizing
blood supply.
Theobroma cacao Cocoa Butter In hair care cocoa butter easily absorbs
into the hair and imparts sheen. It locks in
moisture and helps protect the hair shaft.
Olea Europea Olive Oil In hair care, olive is used for centuries in
hot oil treatments, helps repair split ends,
control dandruff, and makes your hair
shiny, silky, and lustrous
Triticum vulgare Wheat Germ Oil Expeller pressed from the germ of the
wheat kernel is rich in vitamins and
minerals. Virgin wheat germ oil is rich in
vitamin E which acts as natural
antioxidant. In hair care, wheat germ oil
improves the scalp’s ability to utilizeoxygen, leaving the scalp healthy and
softens hair
Butyrospermum
parkii
Shea Nut Butter, In hair care Shea Butter provides deep
nourishment for the hair shaft, and
moisturizes dry, dull hair resulting in
improved luster and manageability. It is
particularly beneficial for processed and
heat-treated hair and is also believed to
help promote new hair growth.
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2.3.4. Evaluation and Quality Control of Shampoo
Several quality control tests are conducted to evaluate the quality of
commercial and prepared formulations. The control tests are including visual
assessments, physicochemical controls conditioning performance tests wereperformed (Ashok and Rakesh, 2010).
One of physicochemical controls is the pH value test which is pH value of
10% v/v shampoo solution in distilled water was measured by using pH meter at
room temperature (Tarun et al., 2014). Most shampoos are formulated as either
neutral or slightly alkaline to minimize the damage to hair. Thus the pH of shampoo
helps in minimizing irritation to the eyes, enhances the qualities of hair and maintain
the ecological balance of the scalp (Baran and Maibah, 1998 Next, foaming ability
was determined by using cylinder shake method while foam stability was evaluated
by recording the foam volume after 1 min and 4 min of shake test (Klein, 2004).
Other than that, dirt dispersion test is an important criterion for evaluation of
cleansing action of shampoo. Shampoos that cause the ink to concentrate in the
foam are considered of poor quality because ink or dirt that stays in foam is difficult to
rinse away and gets re-deposited on the hair (Ali and Kadhim, 2011). Therefore, the
dirt should stay in the water portion for achieving better cleansing action. All
shampoo concentrated the ink in the water portion as it is to ensure the satisfaction
of the shampoo’s cleaning ability and actual effectiveness.
Surface tension test is to indicate the amount of surfactant present in
shampoo. Thus, the amount of surfactant present should be decreases. The
decreases the surface tension influence the increases the cleaning ability of the
shampoo. A shampoo is considered of good quality if it decreases the surface
tension of pure water which is 2.28 until 40 dyn/ cm (Ilton et al., 2007).
The wetting ability of a surfactant is dependent on its concentration and is
commonly used to test its efficacy. The canvas disc method is quick, efficient and
reliable test to evaluate the wetting ability of a shampoo (Manikar and Jolly, 2000).
Meanwhile solid content test is tested in order to indicate where it is hard to wash the
hair. Skin sensitization and Eye irritation are tested in order to avoid any blindness
and chemical hazards affect the consumer.
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2.4.1. Scientific Classification
Each of plants has its own scientific classification. Table 2.1 shows the
Scientific Classification of Aleurites Moluccana.
Table 2.3: The Scientific Classification of Aleurites Moluccana
Domain Eukaryota
Kingdom Plantae
Phylum Spermatophyta
Subphylum Angiospermae
Class Dicotyledonae
Order Euphorbiales
Family Euphorbiaceae
Genus Aleurites
Species Aleurites moluccanus
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2.4.2. Origin and Distribution of Aleurites Moluccana
The exact origin of the Aleurites Moluccana plant is not identified. It was
introduced aboriginally throughout the Pacific Islands and is now a common tree of
the Pacific. This species has been widely introduced to South and Central America,
the Caribbean, Japan and Africa. In the tropical oceanic islands of the Pacific, A.
moluccanus was intentionally introduced as a useful plant by the first Polynesian
migrants at least 1000 years ago and is now widely naturalized (Larrue et al., 2010)
To the Polynesians it is an important cultural tree, and they transported it across
much of South-east Asia and Oceania in prehistoric times as a “canoe plant”. This
ancient transportation makes it difficult to distinguish between the natural range of
the species and the areas where it has been introduced by man. Therefore, there is
some debate as to the limits of its true native range. Its native distribution is reported
as centred on the Indo-Malaysia region, and probably extends from Myanmar and
China throughout the Malay Archipelago, and as east as French Polynesia (PIER,
2013).
As an introduced species, A. moluccanus is now widespread across the
tropics, being found in Bangladesh, Kenya, Uganda, Madagascar, the Comoros,
South Africa, Brazil and many islands in the Caribbean (Elevitch and Manner, 2006;
Oyen, 2007), and has even been planted on isolated oceanic islands such as Pitcairn
and St Helena (Varnham, 2006). In Brazil, it is abundant in southern and south-
eastern states, from São Paulo to Rio Grande do Sul (Quintão et al., 2011). In
Hawaii, A. moluccanus is widespread, and has been designated as the official state
tree (Little and Skolmen, 2003).
2.4.3. Description of Aleurites Moluccana
Aleurites Moluccana is a medium-sized tree reaching 20 m tall with pendulous
branches. It can reach height of up to 90 cm. It has simple leaves, variable in shape,
and is up to 30 cm long. Aleurites Moluccana has a large and has irregular branches
drooping downwards to ground level. The tree is distinctive from a distance (Scott
and Thomas, 2000) due to the silvery green colour of the leaves. The silvery green
colour is due to a thick covering of stellate hairs, which as the leaf ages, it will fade.
The leaves has very unique shaped but also quite variable in gross morphology.
Older leaves and those on higher branches, tend to be a simpler triangular or oval
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shape. Meanwhile, young leaves and leaves on lower branches are often three-lobed
or five-lobed. The leaves are typically 10 cm to 20cm long are arranged alternately
and have wavy margins. There is a pair of glands that produce a sweet secretion
located at the leaf stalk that joins the blade of leaf.
Flowers occur in large clusters and are white or white with red or orange
veins. It is in terminal cymes which each of it is about 10cm to 15cm long. Several
smaller male flowers will be surrounded with one female flower. The female flowers
are up to 13mm long with five separate creamy white petals while the male flowers
are similar to the female flowers but they are longer and thinner.
Based on figure 2.5, the fruit of Aleurites Moluccana is green turning to brown
at maturity. It is hard and round drupes which is about 5 cm to 6 cm long and 5 cm to
7 cm wide. The capsule of Aleurites Moluccana is 2 to 3 inches long and contains
three to seven hard seeds with a white flesh. The unshelled seed looks like an
unshelled hickory nut while the hulled seed looks like a chestnut. The seeds are
contained within a tough black shell that resembles that of a walnut; de-husked
seeds number approximately 100 –120 per kilogram (Elevitch and Manner, 2006).
Figure 2.5: The parts of Aleurites Moluccana fruit.
Aleurites Moluccana has a large geographical distribution. Climatically, it can
tolerate and be found in subtropical dry, wet climates and tropical very dry to wet
forest climates. The elevation range is typically in range 0 m to 700 m in Hawaii
(Elevitch, C.R., and H.I. Manner, 2006). The species is able to withstand mean
maximum temperature of 26 °C to 30 °C and mean minimum temperature of 8 °C to13 °C.
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The plant prefers light and medium texture soils such as sands, sandy loams
and sand clay loams. Besides that, it grows in lightly acidic to alkaline soils which
have pH value of 5 to 8. Meanwhile, in drought the Aleurites Moluccana has quite
tolerant once well establish, however, it flourishes in moist environment (Krisnawati
et al., 2011).
There are few abilities of Aleurites Moluccana tree. Firstly, the tree can grow
well even on relatively poor sites provided ample soil moisture is available during
establishment. Next, the plant regrows well even after severe pruning although it has
a tendency to die after two or more pruning. Lastly, this plant is known for its ability to
grow well on slopes, steep gulches and cliffs (Elevitch, C.R., and H.I. Manner, 2006).
The tree species associated with Aleurites Moluccana vary across its natural
and introduced range. In the Cook Islands, they include the native species
Elaeocarpus floridanus and Hernandia moerenhoutiana and the introduced species
Cocos nucifera, Morinda citrifolia, Hibiscus tiliaceus and Psidium guajava; in French
Polynesia, they include H. tiliaceus and Rhus taitensis on forested slopes, and a
wider range of native species on rocky slopes. In Hawaii, the native species
associated include species of Diospyros and Pisonia, and introduced species include
Syzygium cumini, Schinus terebinthifolia and Eucalyptus species (Elevitch and
Manner, 2006).
2.4.4. Application of Aleurites Moluccana
There are many applications of Aleurites Moluccana species to the society in
different areas. Table 2.4 shows the applications of Aleurites Moluccana species to
the society.
Table 2.4: The Applications of Aleurites Moluccana (Orwa et al, 2009)
Application Usage
Food Technology Aleurites Moluccana is considered edible when the
kernels are roasted and cooked.
After removing the hard outer coat, the seed is pounded
and eaten as a sauce.
Every 100 g, the seed is reported to contain 626 calories,
63 g fat, 19 g protein, 8 g total carbohydrate, 7 g water, 3
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g ash, 200 mg phosphorus, 80 mg calcium, 2 mg iron,
and 0.06 mg thiamine.
Fuel Seed oil is suitable, with modification, for use as a
substitute for diesel, the residues for conversion to
alcohol or pyrolysis.
In Uganda, it is planted as a backyard tree for firewood.
Timber Wood whitish and soft and suitable as a timber species.
Tannin or dyestuff Bark contains about 4 –6% tannin.
Lipids Seed yields 57-80% of inedible, semi-drying oil, liquid at
ordinary temperatures, solidifying at -15 deg. C,
containing oleo stearic acid.
The oil, quicker drying than linseed oil, is used as a wood
preservative, for varnishes and paint oils, as an
illuminated, for soap making, shampoo, waterproofing
paper, insulating material and rubber substitutes.
Oil is painted on bottoms of small crafts to protect
against marine borers; also prevents feeding by striped
cucumber beetle.
The oil is inferior to tung oil, extracted from a related
Chinese species, A. fordii, and used mainly for
varnishing wood.
Commercial production of oil yields 12-18% of the weight
of the dry, unhulled fruits, the fruits being air-dried to
about 12% to 15% mc before pressing. Oil yields as high
as 300 kg/h has been reported.
Poison Seeds are moderately poisonous. The oil cake,
containing about 46% protein is said to be poisonous.
Medicine Bark used to treat tumours in Japan. The oil is purgative
and sometimes used like castor oil.
Kernels are laxative, a stimulant and a sudorific.
The irritant oil is rubbed on scalp as a hair stimulant.
In Malaya, the pulped kernel is used in poultices for
headache, fevers, ulcers and swollen joints.
In Java, the bark is used for bloody diarrhoea or
dysentery.
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Bark juice with coconut milk is used for sprue.
Malayans apply boiled leaves to the body for headaches
and gonorrhoea.
Shade or Shelter The leafy rounded crown provides shade.
Soil improver Seed press cake is suitable as a fertilizer.
Ornamental Aleurites Moluccana is an attractive tree with its cream
white flowers that may appear more than once a year.
Fertilizer The remaining seed cake can be used as fertilizer
2.4.5. Aleurites Moluccana Oil as Remedy
It is stated that the oil extracted from Aleurites Moluccana Seeds have hair
growth promoting properties based on traditional text. Moreover, there are Aleurites
Moluccana oil products available in the market. Hence, the present study is aimed to
the production of hair growth herbal shampoo by using Aleurites Moluccana Seeds
Extracts.
According to Adida Muhammad (2014), A. Moluccana oil contains substantial
amounts of anti-aging component known as omega-3 fatty acids that helps to
strengthen and restore radiance to the hair. Aleurites Moluccana boast one of the
highest concentrations of omega rich oils (omega-3, omega-6 and omega-9), besides
of vitamin A and E as antioxidants that can penetrate into hair scalp and keep hair
looking younger and shinier. Meanwhile, Noviansyah and Sidharta (2009) stated that
A. Moluccana oil is always used as an ingredient for traditional medicine to prevent
hair loss and enhance hair growth. Besides, it also used in modern cosmetic to
enhance hair growth.
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2.5. Extraction Method
Extraction is a separation process consisting in the separation of a substance
from a matrix. It is divided into Liquid-liquid extraction or Solid phase extraction.
Meanwhile, extraction process is a process of extracting active agent, wastesubstance, or plant oil from fruit or herbs. There are a few types of extraction exist
which are solid-liquid extraction, liquid-liquid extraction or gas-liquid extraction
(absorption).
The extraction process can be carried out in a different ways to extract essential
oil such as steam distillation, solvent extraction, ultrasonic extraction, hydro
distillation, Soxhlet extraction, pressure extraction and many more. Soxhlet extraction
had been widely used in industry because of its own advantage which is solventextraction system is faster, less laborious, and consume less amount of solvent than
other conventional methods but it presents low selectivity and require longer time and
heating. Furthermore, the advantage of using solvent extraction is that it greatly
increases the yield of the product. However, all of these organic solvents had their
own difficulties in their availability. In the steam distillation method, there is no solvent
used to extract the material but pure water is the main component to do it (Khairu
Aizam, 2006). Hydro distillation is a method of extraction which is the method is
economically viable and safe (Nurul Azlina, 2004). The disadvantage of using thismethod is that it required higher retention time to extract the sample.
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2.5.1. Ultrasonic –Assisted Extraction
Ultrasonic- assisted Extraction mechanism used sound waves which have
frequencies higher than 20 kHz. Sound waves must travel in a matter and they
involve expansion and compression cycles during travel in the medium. Expansionpulls molecules apart and compression pushes them together. The expansion can
create bubbles in a liquid and produce negative pressure. The bubbles form, grow
and finally collapse. Close to a solid boundary, cavity collapse is a symmetric and
produces high-speed jets of liquid. The liquid jets have strong impact on the solid
surface (Luque-Garcia & Luque de Castro, 2003).
Ultrasonic baths or closed extractors fitted with an ultrasonic horn transducer
are the two general designs of ultrasound-assisted extractors. The mechanical
effects of ultrasound affect a greater penetration of solvent into cellular materials and
improve mass transfer. Ultrasound in extraction can also disrupt biological cell walls,
facilitating the release of contents. Therefore, efficient cell disruption and effective
mass transfer are cited as two major factors leading to the enhancement of extraction
with ultrasonic power (Mason, Paniwnyk, & Lorimer, 1996). In contrast to
conventional extractions, plant extracts diffuse across cell walls due to ultrasound,
causing cell rupture over a shorter period (Chemat, Lagha, Ait Amar, Bartels, &
Chemat, 2004; Li et al., 2004; Toma, Vinatoru, Paniwnyk, & Mason, 2001; Vinatoru,Toma, & Mason, 1999).
Plant characteristic such as moisture content and particle size, and solvent
used for the extraction should be checked in order to obtain an efficient and effective
ultrasound-assisted extraction. Other than that, many factors such as frequency,
pressure, temperatures and sonication time govern the action of ultrasound.
There are few advantages of using ultrasound in solid –liquid extraction
include the increase of extraction yield and faster kinetics. Ultrasound can alsoreduce the operating temperature allowing the extraction of compounds.
Furthermore, the ultrasound-assisted extraction can be used with any solvent for
extracting a wide variety of natural compounds. However, the effects of ultrasound on
extraction yield and kinetics may be linked to the nature of the plant matrix.
Ultrasound-assisted extraction has been used to extract nutraceuticals from
plants such as essential oils and lipids (Chemat et al., 2004; Sharma & Gupta, 2004),
dietary supplements (Albu, Joyce, Paniwnyk, Lorimer, & Mason, 2004, Wu et al.,
2001). An overview of ultrasound-assisted extraction of bioactive compounds from
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herbs was drafted by Vinatoru (2001).Ultrasound can increase extraction
yield. Meanwhile Sharma and Gupta (2004) found that ultra-sonication was a critical
pre-treatment to obtain high yields of oils from almond, apricot and rice bran. The
yield of oil extracted from soybeans also increased significantly using ultrasound (Li
et al., 2004). Besides, the use of ultrasound reduced the extraction at least to half of
the time needed by conventional extraction methods without any change in the
composition of extracted oils (Luque-Garcia & Luque de Castro, 2004). Wu et al,
(2001) found the ultrasound-assisted extraction of ginseng saponin occurred about
three times faster than traditional Soxhlet extraction. Ultrasound-assisted extraction
was considered as an efficient method for extracting bioactive compounds from
Solvia officinalis (Salisova et al. , 1997) and Hibiscustiliaceus L. flowers (Melecchi et
al., 2002), antioxidants from Rosmarinus officinalis (Albu et al., 2004), and steroids
and triterpenoids from Chresta spp. (Schinor, Salvador,Turatti, Zucchi, & Dias, 2004).
2.6. Solvent
Current isolation and chemical purification methods used include solvent
extraction processes that utilize solvent polarity as a major separation technique. The
solvent methods have been broadly classified on the basis of process of extraction.
Amongst separation methods, extraction by using solvent occupies the most
favoured position. During the extraction of an ionically bound lipid, an ion exchange
reaction with available cations must occur. Under some conditions the protein is
pulled into the organic solvent together with its acidic lipid. In samples that content a
relatively large proportion of ionic material (spinal fluid, buffered tissue
homogenates), the cationic composition might affect the ion exchange reaction or
solubility in the organic solvent.
In Ultrasonic- assisted Extraction, solvent is needed to enhance the extractionprocess. Solvent is a liquid that act as the medium for a reaction. Common uses for
solvents are in dry cleaning, paint thinners and in extraction of lipid. Water is a
solvent for polar molecules and the most common solvent which is called as
universal solvent. Solvents have various applications in chemical, pharmaceutical, oil
and gas industries, including in chemical syntheses and purification processes.
There are three polarity-based classes which are polar protic such as water ,
low molecular weight alcohols such as ethanol and methanol, and the solutions of
low molecular-weight carboxylic acids , polar aprotic such as acetone and ethyl
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acetate, and non-polar such as carbon and hydrogen (Reichardt & Welton, 2011).
Ultrasonic behaviour of solvents is considerably affected by their viscosity and also
vapour pressure as in less viscous solvents and low vapour pressure, it can
produced a cavitational bubbles more easily because the ultrasonic intensity applied
can more easily exceed the molecular forces of the solvent. Differences in the
extraction efficiency of various solvents have been attributed to their polarities
(Fernandez-Agullo et al., 2013).
2.6.1. Acetone
Acetone which is a polar solvent can extract the least polar lipids, such as
triglycerides and cholesterol. Significant amounts of other lipids are also removed,
however, so its primary use is in preparative work, where a 100% yield is
unnecessary. Acetonitrile is a good solvent however it is rather expensive.
One of example of usage of acetone in extraction process is as acetone has
often been used to convert a wet tissue to a dry powder that can then be extracted
with a relatively small amount of a more polar solvent. It is because of its high
volatility and miscibility with water.
Acetone has a long history of use in extracting lipids without denaturing
proteins since many of the early enzyme isolation methods used a preliminary
dehydration step. Although the extract contains all the tissue water and significant
amounts of other lipids, selective extraction of relatively nonpolar lipids by acetone is
easy. In a typical procedure (Stein and Smith, 1982), the tissue was homogenized
with 10 volume of cold acetone, filtered, and air-dried. The powder was then
extracted with 5 volume of cold acetone and the two filtrates were pooled. Water can
be removed by codistillation with toluene or hexane or by partitioning with hexane
after much of the acetone has been removed by rotoevaporation. The polar lipids in
the tissue residue can be extracted relatively effectively with only a small volume of
polar solvent. Besides, the most suitable solvents to extracts oil are polar solvent
such as ethanol, methanol, ethyl acetate and more (Yu et al, 2010). Other than that,
Acetone extracts more oil from cottonseed than hexane (Lester, D and Greenberg
L.A., 1951)
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CHAPTER 3
METHODOLOGY
3.1. An Overview
In this chapter, methods involved in the experiment are discussed including
the preparation method and how the experiment is being conducted where the
procedure are split into few parts which is preparation of Aleurites Moluccana Seeds,
extraction of Aleurites Moluccana Seeds by using Ultrasonic bath, the formulation of
Hair Growth Herbal Shampoo and the formulated shampoo with marketed shampoo
will undergo evaluation and quality testing. The detail procedure and process flow will
be explained and were addresses in this chapter.
3.2. Methodology Overview
Figure 3.1 The overview of methodology of Production of Hair Growth Herbal
Shampoo by using Aleurites Moluccana Seeds Extracts
Preparation of Aleurites Moluccana Seeds
Extraction of Aleurites Moluccana Seeds
Formulation of Hair Growth Herbal Shampoo
Evaluation and quality testing
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3.3. Materials
The materials needed for extractions of Aleurites Moluccana seeds are
solvent and Aleurites Moluccana Seeds. The solvent used for this production is
Acetone purchased from Hmbg Chemicals. The grade of solvents is analytical grade(Sebah, 2007).
Figure 3.2 shows the raw material used for formulation of shampoo are
Aleurites Moluccana seeds extract, Cocamide DEA, Cocamidoproply Betaine,
Formaldehyde, and Ethylenediaminetetraacetic acid (EDTA) Disodium, Sodium lauryl
sulfate (SLS), Sodium Chloride, Sodium Hydroxide, and Citric Acid.
Figure 3.2 The raw material used for formulation of shampoo
3.4. Equipment
The equipment used in the methodology is B204-S Mettler Toledo, USA
analytical balance which is to measure the weight of sample and the formulations.
Based on figure 3.3, the Ultrasonic Bath from brand D-78224 Singan/Htw Elma is
used for extraction of oil from Aleurites Moluccana Seeds by using Acetone as
solvent and water as heating medium.
The equipment used for preparation, extraction of Aleurites Moluccana Seeds
and evaluation and quality control tests are drying oven, rotary evaporator (Figure
3.4), pH meter (Mettler Toledo, USA) and Brookfield Viscometer (Model DV-I Plus,
LV, USA).
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Figure 3.3 Ultrasonic Bath from brand D-78224 Singan/Htw Elma
Figure 3.4 Rotary Evaporator
3.5. Procedures
The procedure is started with preparation of Aleurites Moluccana Seeds.Next, the procedures proceed with the extraction of Aleurites Moluccana Seeds by
using Ultrasonic bath. Then, the formulation of Hair Growth Herbal Shampoo is
formulated and the formulated shampoo with marketed shampoo will undergo
evaluation and quality testing.
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3.5.1. Preparation of Aleurites Moluccana Seeds
The preparation of Aleurites Moluccana Seeds are needed in order to prepare
the sample before undergo the extraction process. Firstly, the kernels of candle nut
seed are removed from hard skin. It is cut into small pieces about 0.5 cm to 1 cm.Then it is grind by using domestic blender and sieved to get uniform size (Adida
Muhammad, 2014). Based on figure 3.5, the grind seeds will be dried to completely
remove its moisture content by using laboratory oven at 60 °C for about 24 hours
(Divya et al, 2013). Then the sample is weight by using analytical balance according
to the require mass which is 150 g. As seen in figure 3.6, the sample is ready to be
used for extraction process.
Figure 3.5 Removal of moisture content in Aleurites Moluccana Seeds
Figure 3.6 shows the blended Aleurites Moluccana Seeds
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3.5.2. Extraction of Aleurites Moluccana Seeds
Extraction process is the process to extracts oils from the Aleurites
Moluccana seeds. The extraction process involved Ultrasonic Extraction Method.
Ultrasonic Extraction Method is a method which is the ultrasonic wave generatessupersonic liquid micro jet that has ability to disrupt plant cells when the cavitating
bubbles collapse at close proximity. In contrast to conventional extractions, plant
extracts such as Aleurites Moluccana Seeds diffuse across cell walls due to
ultrasound, causing cell rupture over a shorter period (Chemat, Lagha, Ait Amar,
Bartels, & Chemat, 2004; Li et al., 2004; Toma, Vinatoru, Paniwnyk, & Mason, 2001;
Vinatoru, Toma, & Mason, 1999).
Approximately, 25 g of A. Moluccana seeds is mix with 250 ml of the extraction
solvents (acetone) into a beaker which is 1:10 plant materials: solvent proportion, at
room temperature (Quintão et al., 2011). Then, mixture is stirred until the solution mix
well in fume cupboard as shown in figure 3.7.
Figure 3.7 The mixed Aleurites Moluccana seeds and solvent solution
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Figure 3.8 The mixed Aleurites Moluccana seeds and solvent solution is immersed in
ultrasonic bath.
Based on figure 3.8, the ultrasonic irradiation experiments will be carried out in a
sonomatic cleaning bath operating at 80W power and 40 kHz frequency. Dimensions
of the tank are 2100 cm3. The sample beakers are immersed into the ultrasonic bath
for irradiation under extraction conditions including time (30 min), mass (25 g) and
solvents (250 ml of acetone). Finally, the extracts are filtered by using Whatman
paper #3 and the solvents are removed by using a rotary evaporator, BUCHI V-850.
These procedures are repeated in order to achieve 15 g of Aleurites Moluccana Oil
extracted.
3.5.3. Filtration Process
Filtration is a mechanical or physical process to separate the solid
particulates from fluids or solution. However, filtration process is a process ofseparation of solids from suspension in a liquid which means of a porous medium or
screen that retains the solids and allows the liquid to pass (Gauri S. Mittal, 1997).
Based on figure 3.9, the apparatus prepared for the filtration process are
conical flask, filter funnel and filter paper. The filter paper which is Whatman paper #3
is fold into triangular shape and placed in the filter funnel. The filter funnel contained
filter paper for filtration is poured with a beaker filled with sample submerges with
solvent. After a while, the extracted product containing extracts of Aleurites
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Moluccana and remaining solvent was collected in the conical flask. Next, the
extracted product is transferred into the sample flask to undergo Rotary Evaporator.
Figure 3.9 The filtration process of Aleurites Moluccana seeds and remaining mixed
solvent and oil extracted
3.5.4. Rotary Evaporating Process
Rotary Evaporator is an equipment to separate the extracts of Aleurites
Moluccana and solvent from the mixture of both. The sample flask is placed in water
bath under the reduced pressure and heating with the rotation of sample flask to
ensure the solvent in the bottle spread and evaporated. The temperature set for the
water bath of Rotary Evaporator is 56 °C at 760 mmHg (Lide, 2006). The solvent is
vaporizing because of its low boiling point compared to the boiling point of extracted
oil from the sample. The solvent will be suck through vacuum system by reduce
pressure and is transferred to the condenser with coil passing coolant into which
coolant mixtures. Solvent after it re-condenses is flow to the condensate-collecting
flask at bottom of the condenser. The sample that contained the oil extracted from
Aleurites Moluccana Seeds is left at the sample flask. It is then transferred into glass
bottle for analysis. The solvent left will be dispose into solvent waste container.
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3.5.5. Formulation of Hair Growth Herbal Shampoo
Herbal ingredients in the formulation are viable alternative to synthetic
shampoo. About 100 hair growth products are available in the markets which are
prepared by combination of one or more herbal ingredients (Thakur R, 2015). Although herbal ingredients are currently widely accepted by the patient, the scientific
review among dermatologists is limited. Table 3.1 shows the formulation of herbal
shampoo.
Table 3.1 The formulation of herbal shampoo (The Lubrizol Corporation, 2013)
Material Weight (%) Function
Deionized Water 60.00 Diluent
Sodium Lauryl Sulfate (28
wt. %)
17.95 Surfactant
Cocamidopropyl Betaine
(30 wt. %)
5.00 Surfactant
Cocamide DEA (88 wt. %) 0.60 Surfactant
Aleurites Moluccana Seeds
Extracted Oil
15.00 Hair growth promoter
agent
Disodium EDTA 0.05 Chelating agent
Formaldehyde 0.4 Preservative
Sodium Hydroxide - Neutralizer (pH adjuster)
Sodium Chloride - Viscosity adjuster
Citric Acid - Neutralizer (pH adjuster)
Basil Essential 1.0 Fragrance
Firstly based on figure 3.10, 60 grams deionized water is mixed with 20
grams of Sodium Lauryl Sulfate (SLS) to dilute the surfactants until uniform in the
main batch of hot plate. Based on 3.11, 5 grams of Cocamidopropyl Betaine, 0.6
grams of Cocamide DEA and 15 grams of sample that contained Aleurites
Moluccana Seeds Extracted Oil are mixed until uniform and it is added into the main
batch to homogenize all the surfactants. In separated vessel, EDTA is dissolved in
deionized water and added to the main batch until uniform. Next, the 0.4 grams of
formaldehyde is added as preservatives and 1 grams of sodium hydroxide or citric
acid is added as neutralizer. Lastly, after all ingredients are mixed well in the main
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batch, it is transferred to bottle. Sodium chloride is added to the formulation as it is
function as viscosity adjuster.
Figure 3.10 The overview of formulation of herbal shampoo
Figure 3.11 The mixing of the ingredients of the formulations
Deionized water is
added to SLS as
diluent in the
main batch.
Cocamidopropyl Betaine,
Cocamide DEA and Aleurites
Moluccana oil is added until
homogenized in another
vessel.
Dissolve EDTA
in deionized
water
Mixed in the main batch and
formaldehyde is added as
preservatives
Sodium Hydroxide or Citric Acid
is added to adjust the pH value
to 5.5-6.5 and mix until uniform
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3.5.6. Shampoo Evaluation Process
A quality control tests including organoleptic and physicochemical
characterization such as pH, solid contents and viscosity were performed in order to
evaluate the prepared formulations. The purpose of quality control tests is to ensurethe quality of the products, specific tests for shampoo formulations including foam
volume and foam stability, eye irritation and skin sensitization tests were also carried
out. The results were compared with frequently used marketed herbal extracts
shampoo (Follow Me) that was considered as reference.
3.5.6.1. Physical appearance/visual inspection
The formulated shampoo and commercial herbal extracts shampoo were
observed for their physical visual inspection. The prepared formulations were
evaluated in terms of their clarity, foam producing ability and colour.
3.5.6.2. Determination of pH value
Based on figure 3.12, the pH of shampoo solution (10% w/v) in distilled water
was determined at room temperature (Griffin JJ, 1977). The pH was measured by pH
meter (Mettler Toledo, USA).
Figure 3.12 The determination of pH value of shampoo by using pH meter
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3.5.6.3. Percentage of solid contents
Four grams of the prepared shampoo were placed in a clean dry evaporating
dish. The weight of the dish and shampoo was determined by using analytical
balance. Based on figure 3.13, the liquid portion of the shampoo was evaporated byplacing on a hot plate and the weight of the shampoo solid contents after complete
drying was determined.
Figure 3.13 The solid content test on the shampoo
3.5.6.4. Wetting time
The canvas was cut into 1-inch diameter discs having an average weight of
0.44 g. The disc was floated on the surface of shampoo solution 1% w/v and the
stopwatch started. The time required for the disc to begin to sink was measured
accurately and noted as the wetting time.
3.5.6.5. Rheological property
The viscosity of the prepared formulations was measured at room
temperature using Brookfield Viscometer (Model DV-I Plus, LV, USA) fitted with a
spindle type 3 while set at spindle speeds of 5 rpm. The temperature and sample
container’s size is kept constants during the evaluation. All measurements were
performed in triplicate at room temperature and the viscosity profile of the shampoos
was measured. The steps are repeated by using 10 rpm and 20 rpm speeds.
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3.5.6.6. Foam, volume and stability
5 ml of the 1% herbal shampoo is put into a 25 ml graduated measuring
cylinder. Then, the measuring cylinder is covered with hand and shaken for 10 times.
The total volumes of foam content after 1 minute shaking and the volume of foam atintervals of 4 minutes is recorded.
3.5.6.7. Eye irritation test
1% of shampoo is dripped into the eyes of the lab rat. The progressive
damage to the rat’s eyes was recorded at specific intervals over an average period of
five minutes. Reactions to the irritants can include swelling of the eyelid, inflammation
of the iris, bleeding and blindness (Barenett G., 1951)
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CHAPTER 4
DISCUSSIONS
4.1. An Overview
All the data obtained from the study are clearly tabulated in this chapter.
Then, the presented results are discussed thoroughly in specific where quality control
tests such as the pH value, solid contents and viscosity, foam volume and foam
stability and eye irritation tests were also carried out. The results were compared with
frequently used marketed herbal extracts shampoo (Follow Me) that was considered
as reference.
The objective of this research is to study the process of extraction of Aleurites
Moluccana Oil by using Ultrasonic-Assisted Extraction, to study the production of hair
growth herbal shampoo by using formulation gathered and to study the quality testing
and analysing the product from formulated hair growth herbal shampoo by using
Aleurites Moluccana Seeds Extracts.
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4.2. Process of extraction of Aleurites Moluccana
Cold pressing, solvent extraction, and different distillation techniques are
stereotypical processes for obtaining oils from plant material (Lago et al., 2014).
However, there are several disadvantages of using the techniques as the usage of
volatile and hazardous solvents, low yields, long extraction times, and high energy
consumption (Zu et al., 2012).
According to Tongnuanchan and Benjakul(2014), the extraction method is
one of the prime factors that determine the quality of oils thus the use of new
extraction techniques for natural substances, which typically use less solvent and
energy, such as supercritical fluid extraction, ultrasound extraction, microwave
assisted extraction, and sub-critical water extraction are being evaluated.
Among these emergent technologies, the ultrasonic assistance extraction
method can accelerate the penetration of solvent and releasing the component from
the cell into the solvent by using sonification. Thus it increase extraction process
(Tian et al., 2013).
4.2.1. Sample Preparation
Based on figure 4.1, the kernels of Aleurites Moluccana seed is removed and
cut into small pieces. Then, the seeds can be powdered and dried before extraction
process. The reason behind the seeds to be cut and powdered is because of to
increase the surface area (Smothers, 2013). Meanwhile the grind seeds will be dried
completely by using laboratory oven at 60 °C for about 24 hours as to remove the
seed extracts’ moisture content (Divya et al, 2013). The sample is dried for time
retention of 24 hours to ensure the moisture content is eliminated accurately.
Figure 4.1 Aleurites Moluccana Seeds after undergo the sample preparation
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process. Meanwhile, 30 minutes sonication time is considered carefully as excess
sonication can damage the quality of extracts (Wang, 2006). Hence, it should be
noted that since ultrasound generates heat, it is important to accurately control the
extraction temperature and time (Salisova, 1997).
4.2.3. Filtration and Rotary Evaporating Process
Filtration process is a process of separation of solids from suspension in a
liquid which means of a porous medium or screen that retains the solids and allows
the liquid to pass (Mittal, 1997).
In this study, filtration process is the separation of Aleurites Moluccana seeds
and a mixture of acetone with Aleurites Moluccana oil from the mixture of both in a
solution. The solution of acetone with the oil is needed for the next process
meanwhile the Aleurites Moluccana seed is thrown into solid waste container.
Next, the main function of Rotary Evaporator is to separate the extracts of
Aleurites Moluccana and solvent from the mixture of both. The sample flask is placed
in water bath under the reduced pressure and heating with the rotation of sample
flask is due to ensure the solvent in the bottle spread and evaporated. The
temperature set for the water bath of Rotary Evaporator is 56 °C at 760 mmHg (Lide,
2006) to avoid acetone vaporize to the air as it is the boiling point of acetone.
Based on figure 4.2, it shows the sample of Aleurites Moluccana oil in the
glass bottle. At first, after rotary evaporating process, the sample that contained the
oil extracted from Aleurites Moluccana Seeds is left at the sample flask. It is then
transferred into glass bottle for analysis. The solvent left will be dispose into solvent
waste container meanwhile the oil extracted from Aleurites Moluccana Seeds is
poured into glass tube for storage. Based on 4.3, the weight of oil extracted is
weighted in order to obtaining minimum of 15 grams for the formulation of hair growth
herbal shampoo.
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Figure 4.2 The sample of oil extracted
Figure 4.3 The weight of oil extracted after three times repeat the procedure of
extraction method.
4.3. Production of Hair Growth Herbal Shampoo
Shampooing is the most common form of hair treatment. The primary function
of formulated hair growth herbal shampoo in this study is associated with specific
problem which is hair loss (Alopecia). The targeted form of shampoos is in liquid like
preparations.
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4.3.1. Formulation of Hair Growth Herbal Shampoo
Based on table 4.1, the targeted weight of product is 100 grams. The
materials which are 60 grams of deionized water, 17.95 grams of Sodium Lauryl
Sulfate, five grams of Cocamidopropyl Betaine, six tenths grams of Cocamide DEA,
15 grams of Aleurites Moluccana Seeds Extracted Oil, five hundredths grams of
Disodium EDTA, four tenths grams of Formaldehyde, one gram of basil oil, sodium
hydroxide, citric acid and sodium chloride.
Table 4.1The formulation of herbal shampoo (The Lubrizol Corporation, 2013)
Material Weight (%) Function
Deionized Water 60.00 Diluent
Sodium Lauryl Sulfate (28
wt. %)
17.95 Surfactant
Cocamidopropyl Betaine
(30 wt. %)
5.00 Surfactant
Cocamide DEA (88 wt. %) 0.60 Surfactant
Aleurites Moluccana SeedsExtracted Oil
15.00 Hair growth promoteragent
Disodium EDTA 0.05 Chelating agent
Formaldehyde 0.4 Preservative
Sodium Hydroxide - Neutralizer (pH adjuster)
Sodium Chloride - Viscosity adjuster
Citric Acid - Neutralizer (pH adjuster)
Basil Essential 1.0 Fragrance
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4.3.2. Process of Production of Hair Growth Herbal Shampoo
The process is started with 60 grams deionized water is mixed with 20 grams
of Sodium Lauryl Sulfate (SLS). This is due to dilute the surfactants until uniform in
the main batch of hot plate of temperature 50 °C which increase the process of
homogenization of the formulated shampoo materials. Other than that, the
importance of the surfactants to be homogenized is to dilute high active surfactants,
produce a stable emulsions and reducing the particle sizes (Deb Shecter, 2015). The
deionized water is used in the process as deionized water did not contain ion that
insoluble with the ingredient used in formulation of shampoo. The