Professional Documents
Culture Documents
SEPTEMBER 2015
SEPTEMBER 2015
ii
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 shampoos 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 evaluations 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.
iii
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.
iv
APPROVAL PAGE
I have Supervised and examined this report and verify that it meets the programmed
and University requirements for the Diploma in Chemical Engineering Technology
(Process).
Date:
Signature:
Supervisors Name: Marmy
Roshaidah binti Mohd Salleh
Official Stamp
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
Date
19 December 2015
vi
vii
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.
viii
TABLE OF CONTENTS
TITLE
PAGE
TITLE PAGE
ii
ABSTRACT
iii
ABSTRAK
iv
APPROVAL
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
1.2
Problem statement
1.3
Objectives
1.4
Scope of study
1.5
Thesis Layout
An overview
2.2.
2.3.
Shampoo
10
11
13
14
ix
2.4.
2.5.
2.6.
17
Aleurites Moluccana
18
19
20
20
22
24
Extraction Method
25
26
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
32
33
34
35
36
38
3.5.6.1.
38
inspection
3.5.6.2.
Determination of pH value
38
3.5.6.3.
39
3.5.6.4.
Wetting time
39
3.5.6.5.
Rheological property
39
3.5.6.6.
40
3.5.6.7.
40
An overview
41
4.2.
42
42
43
44
4.3.
45
46
47
Shampoo
4.3.3. Hair Growth Herbal Shampoo by using
48
49
50
51
52
53
54
56
57
Conclusion
59
5.2.
Recommendations
60
60
60
60
REFERENCES
61
APPENDICES
65
xi
LIST OF TABLES
TABLE NO
TITLE
2.1
PAGE NO
different alopecia
2.2
The Common Herbs used which benefits the hair with its
15
functions
2.3
19
2.4:
22
3.1
36
4.1
46
4.2
49
4.3
54
4.4
56
xii
LIST OF FIGURE
FIGURE NO
TITLE
PAGE
2.1
2.2
2.3:
14
2.4
18
2.5:
21
3.1
3.2
30
3.3
31
3.4
Rotary Evaporator
31
3.5
3.6
32
3.7
33
xiii
solution
3.8
3.9
3.10
35
3.11
37
3.12
3.13
39
4.1
4.2
45
4.3
4.4
48
50
4.6
51
4.7
52
4.8
53
4.9
55
4.10
56
xiv
4.11
4.12
4.13
4.14
xv
LIST OF APPENDICES
APPENDIX
TITLE
PAGE
Viscosity Calculation
81
xvi
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 30s 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 many
properties 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 shampoos formulation.
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, hormonal
factors, 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.
1.3.
Objectives
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.
1.5.
Thesis Layout
i.
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.
i.
iv.
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.
condition 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.
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)
Descriptions
Androge-
nic
evidenced therapies are oral finasteride and topical minoxidil for male
alopecia
Alopecia
areata.
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.
Sensesc-
Also termed senile alopecia, this is a relatively new hair loss category
ent
that recognizes the inevitable effects of the aging process on the hair
Alopecia
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.
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 for
treating 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)
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 the
hair 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.
10
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. (Treb, 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 formulas 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
12
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).
14
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
Sapindus
Common name
Function
Soapnuts
mukorrosi
Hibiscus sabdariffa
Hibiscus
Acacia concinna
Shikakai
Prunus dulcis
Almond Oil
Cera alba
Beeswax
Amla
Theobroma cacao
Cocoa Butter
Olea Europea
Olive Oil
Triticum vulgare
which
acts
as
natural
for
the
hair
shaft,
and
16
17
2.4.
Aleurites Moluccana
Aleurites Moluccana (L.) Willd is a member of Euphorbiaceous family. Some
of common names of the plant are candleberry, candlenut tree, Indian walnut, kukui,
kukui nut and varnish tree. Aleurites Moluccana is originated and native to China,
Taiwan, the Indian sub-continent, south-eastern Asia and northern Queensland. It is
widely grown in Hawaii as Kukui is considered a symbol of peace, protection, and
enlightenment. Due to its multiple uses, the Aleurites Moluccana tree has been
designated as the state tree of Hawaii (Elbert L. Little Jr. and Roger G. Skolmen,
2003). Although the raw fruit of Aleurites Moluccana is poisonous, the fruit of the tree
can be prepared as a food source and has been used in traditional medicinal
treatments. The tree fruit contains flammable oil, up to 70% by content. The tree
derives its name from the fact that the fruit can be burned like a candle. The
Hawaiians also extracted the oil from the tree fruit and burned it in a stone oil lamp
with a cloth wick (Roger G. Skolmen, 2003). It is a medium to large sized ornamental
tree that will grow to a mature height of 50 to 80. Aleurites Moluccana Tree may
develop wide spreading or pendulous branches. The trees prefer moist, but well
drained soils and grow best in full sun or light shade. A benefit of planting an
Aleurites Moluccana tree is the spring display of flowers. The tree will display an
abundance of fragrant, white flowers in the spring. Figure 2.4 shows fruit branch of
Aleurites Moluccana tree.
18
Eukaryota
Kingdom
Plantae
Phylum
Spermatophyta
Subphylum
Angiospermae
Class
Dicotyledonae
Order
Euphorbiales
Family
Euphorbiaceae
Genus
Aleurites
Species
Aleurites moluccanus
19
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 100120 per kilogram (Elevitch and Manner, 2006).
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).
Usage
22
Timber
Tannin or dyestuff
Lipids
-15 deg.
C,
Poison
Seeds
are
moderately
poisonous.
The
oil
cake,
Shade or Shelter
Soil improver
Ornamental
Fertilizer
24
2.5.
Extraction Method
Extraction is a separation process consisting in the separation of a substance
25
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
26
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 signicantly 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,
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 extraction
process. 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
27
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)
28
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
29
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.
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).
30
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.
31
32
Figure 3.7 The mixed Aleurites Moluccana seeds and solvent solution
33
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.
34
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
35
Weight (%)
Function
Deionized Water
60.00
Diluent
Surfactant
wt. %)
Cocamidopropyl
Betaine 5.00
Surfactant
(30 wt. %)
Cocamide DEA (88 wt. %)
0.60
Surfactant
Hair
Extracted Oil
agent
growth
promoter
Disodium EDTA
0.05
Chelating agent
Formaldehyde
0.4
Preservative
Sodium Hydroxide
Sodium Chloride
Viscosity adjuster
Citric Acid
Basil Essential
1.0
Fragrance
36
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
37
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 ensure
the 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.
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).
38
3.5.6.3.
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 by
placing on a hot plate and the weight of the shampoo solid contents after complete
drying was determined.
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
39
3.5.6.6.
3.5.6.7.
1% of shampoo is dripped into the eyes of the lab rat. The progressive
damage to the rats 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)
40
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.
41
4.2.
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
42
44
Figure 4.3 The weight of oil extracted after three times repeat the procedure of
extraction method.
4.3.
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.
45
Weight (%)
Function
Deionized Water
60.00
Diluent
Surfactant
wt. %)
Cocamidopropyl
Betaine 5.00
Surfactant
(30 wt. %)
Cocamide DEA (88 wt. %)
0.60
Surfactant
Hair
Extracted Oil
agent
growth
promoter
Disodium EDTA
0.05
Chelating agent
Formaldehyde
0.4
Preservative
Sodium Hydroxide
Sodium Chloride
Viscosity adjuster
Citric Acid
Basil Essential
1.0
Fragrance
46
47
Figure 4.4 Final product of hair growth herbal shampoo by using Aleurites
Moluccana seed extracts
48
4.4.
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 ensure the 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. Based on table 4.2, it shows overview of results for
each shampoo evaluation process.
Table 4.2 The overview results for Shampoo Evaluation Process
Shampoo
Formulated
hair
growth Commercial
hair
growth
Evaluation criteria
Physical
Milky cream
Light green
appearance
Foam
Good foaming
ability
pH value
5.52
6.95
20.77
content (%)
Wetting time (s)
177
132
26
(millilitre)
Eye irritation test
Irritation
Mild irritation
49
4.4.1.
observed for their physical visual inspection. The prepared formulations were
evaluated in terms of their clarity, foam producing ability and colour. Based on figure
4.5, it shows that the colour of formulated hair growth herbal shampoo produced is
milky cream and the foam producing ability is mild foaming. Meanwhile, for Follow
Me shampoo (figure 4.6) shows a light green colour and good foam producing ability.
50
4.4.2. Determination of pH
The pH of shampoo formulations is important to improve and enhance the
qualities of hair, minimize the irritation to the eyes and stabilize the ecological
balance of the scalp (Hart Jr, 1980). The measurement of pH value of shampoo is
measured after the pH meter is cleaned properly to avoid any disrupted results. The
pH of shampoo solution 10% in distilled water was determined at 25 C and the
results are presented in Table 4.2.
Nowadays it is a trend to promote shampoos of lower pH as it is one of the
ways to minimize damage to the hair. This is because mild acidity prevents swelling
and promotes tightening of the scales, thereby inducing sheen. As seen from figure
4.6, formulated hair growth herbal shampoo shows a lower pH than Follow Me, but
was ranged 5.5 to 7.0. This is because when the pH of the hair gets too high, the hair
becomes too alkaline, and the cuticles open, the hair becomes dry and brittle, and
the shine disappears (Neeharika Rallapally Et. al, 2013).
pH value
6
5
4
6.95
5.52
2
1
0
Formulated hair growth herbal
shampoo by using Aleurites Moluccana
seed extracts
Type of shampoo
51
21
20.75
20.77
20.7
20.65
52
177
132
Type of shampoo
Viscosity (mPa.s)
Formulated Hair Growth
Follow Me
Herbal Shampoo
5
600.0
1800.0
10
550.0
1767.0
20
116.5
225.0
54
Viscosity (mPa.s)
1600
1400
1200
1000
800
1800
1767
600
400
200
600
550
116.5225
0
5
10
20
55
Volume of foam of
Volume of foam of
Follow Me shampoo
(ml)
29
26
28
26
26
26
24
26
24
26
30
25
Volume of foam of
formulated hair growth
herbal shampoo (ml)
20
15
29 27
26 26
24 26
24 26
10
5
0
Time intervals (minute)
In this case, the time of foam productivity and its stability should be
considered too. Foam stability prevents replacement of removed germs from the hair.
Therefore, the procedures are conducted for 4 minutes in order to obtained precise
measurement of foam stability.
Based on figure 4.10, it shows that Follow Me shampoo shows good stability
compared to formulated hair growth herbal shampoo. Hence, the formulated
shampoo has more foam productivity but lower stability than its commercial
shampoo.
Figure 4.11 Eye of lab rat specimen before treatment with formulated hair growth
herbal shampoo
57
Figure 4.12 Eye of lab rat specimen after treatment with formulated hair growth
herbal shampoo
Figure 4.13 Eye of lab rat specimen before treatment with marketed shampoo
Figure 4.14 Eye of lab rat specimen before treatment with marketed shampoo
58
CHAPTER 5
5.1.
Conclusion
Hair Loss (Alopecia) often presents suddenly with loss of the hair at the follicle
and affects most people of all range of age and gender. There are few factors that
contributed which are aging process and genetics factor. It is often psychologically
debilitating and does not have a cure. However there are treatments that can
regrowth the hair by shampooing. 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 shampoos 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 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. Meanwhile, most of
shampoo evaluations 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.
59
5.2.
Recommendations
There are few recommendations suggested in order to produce better
60
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64
APPENDICES
+ +
3
Dial reading
Formulated Hair Growth
Follow Me
Herbal Shampoo
First
Second
Third
First
Second
Third
reading reading
reading
3.00
3.10
3.00
9.10
9.00
9.00
10
5.50
5.45
5.50
17.60
17.70
17.70
20
2.43
2.18
2.38
4.5
4.55
4.6
Table below shows the average dial reading of three repeated measurement
Spindle speed (RPM)
Follow Me
Herbal Shampoo
5
10
5.5
17.67
20
2.33
4.5
65
Viscosity (mPa.s)
Formulated Hair Growth
Follow Me
Herbal Shampoo
5
3 x 200 = 600.0
9 x 200 = 1800.0
10
20
2.33 x 50 = 116.5
4.5 x 50 = 225.0
66