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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

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