FORMULATION &

EVALUATION OF
SHAMPOO
Dr. Gitika Dhingra
Assistant Prof
NCRD’s Sterling Institute of
Pharmacy, Nerul, Navi Mumbai
Shampoos, contd…
Outline

• Introduction
• Product Ingredients
• Manufacturing Process
• Evaluation of Shampoos
• Myths about shampoo usage
• References
 A shampoo is a preparation of a
surfactant (i.e. surface active
material) in a suitable form – liquid,
solid or powder – which when used
under the specified conditions will
remove surface grease, dirt, and skin
debris from the hair shaft and scalp
without adversely affecting the user.
Introduction, contd…
Why Shampoos are needed???

1. Completely remove dirt

2. Protect the hair
3. Soothe the scalp skin
4. Treat dandruff, lice or other
scalp problems
4
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Introduction, contd…
How Shampoos work??

5
 Formulation Parameters

viscous liquids

clear or opaque
Shampoo

Containing 20–40% solids

pH 5.5
viscosities 500–1500 centipoise

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 Formulation Ingredients

a) Water
Raw Materials

b)Surfactants
(Foam Boosters and
Stabilizers)

7
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 Formulation Ingredients

c) pH adjusters
Raw Materials

d) Viscosity modifiers

e) Sequestering Agents

8
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 Formulation Ingredients

f)Opacifiers
Raw Materials

g)Conditioning Agents

h) Anti-dandruff Agents

9
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 Formulation Ingredients

j)Perfumes
Raw Materials

k)Colors

L)Preservatives

10
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Formulation Ingredients, contd…
Water

This is the main ingredient in all shampoo

preparations, comprising about 60-80%
of the solution. It aids in diluting the
cleaning agents, thereby reducing
irritation. It makes the shampoo formula
easier to spread on the hair and scalp.
Formulation Ingredients, contd…
Surfactants
Surfactants are compounds that lower the
interfacial tension of a between two phases.
These are molecules that possess both
hydrophillic and lipophillic moieties in their
structure. they get adsorbed on the interface and
helps the phases to misciblize.

1. Principal surfactants: Provide detergency and

foam.
2. Secondary surfactants: Improve detergency, foam
and hair condition.
Formulation Ingredients, contd…
Surfactants
• Anionic surfactants are mostly used (good foaming
properties). The hydrophilic portion carries a negative
charge which results in superior foaming, cleaning and
end result attributes.
• Non-ionic surfactants have good cleansing properties
but do not have sufficient foaming power.
• Cationic surfactants are toxic and are hence not used.
However, they may be used in low concentration in hair
conditioners.
• Ampholytics, being expensive, are generally not used.
However, they are mainly used as secondary
surfactants and good hair conditioners.
Formulation Ingredients, contd…
SLES is preferred over SLS
Sodium Lauryl Sulfate (SLS) and Sodium
Lauryl Ether Sulfate (SLES) play similar
role in shampoos. SLS is a skin, eye and
respiratory tract irritant (Environmemt
Canada has categorized it as inherently
toxic to aquatic organisms). To make it
less irritating, it is ethoxylated (by adding
ethylene oxide), resulting in SLES.
 Formulation Ingredients, contd…
Foaming Agents
• These agents are used to introduce gas bubbles into the
water. The foam, also known as lather, is important, as it
functions to spread the detergent over the hair and scalp, but
it does not participate in cleaning.
• It is true that a shampoo applied to dirty hair will not foam as
much as the same shampoo applied to clean hair. This is due
to the sebum inhibiting bubble formation. Thus, a shampoo
will foam less on the first shampooing and more on the
second shampooing.
• Some of the prescription corticosteroid shampoos do not
foam as much as cosmetic shampoos, but this does not mean
their cleaning is inadequate.
• Examples: Lauroyl monoethanolamide, sarcosinates
Formulation Ingredients, contd…
pH Adjusters

These agents are used to prevent the hair

shaft from alkalinization. Most detergents
are having alkaline pH, which causes hair
shaft swelling. This swelling loosens the
protective cuticle predisposing the hair
shaft to demage.

Example: Citric acid, Glycollic acid

Formulation Ingredients, contd…
Thickening Agents

These agents are used shampoo thick and

creamy. Thickening may be achieved by
adding salts or gums. Gums improve
viscosity because of their gel-like
properties.

Eg:Tragacanth gum, Gum Karaya, Carboxy

methyl cellulose.
 Formulation Ingredients, contd…
How salt act as thickening agent for
shampoos containing anionic surfactant
• The viscosity of the shampoo solution depends on
the size and packing structure of micelles (tiny
vesicles of surfactants).
• In general, higher charge density causes the
micelles to repel and result in a thinner solution.
• The sodium ions from the salt lower the charge
density of the micelle surface. This makes them
more able to pack closer together and creates a
thicker solution.
Formulation Ingredients, contd…
Sequestering Agents

These are the agents to chelate magnesium

and calcium ions, present in hard water,
preventing formation of insoluble soaps
(scum). This scum film will make hairs look
dull and may contribute to itching and
symptoms of seborrheic dermititis.

Eg:EDTA
Formulation Ingredients, contd…
Opacifying Agents

• Chemical agents added to the preparation

to make it opaque, so that light does not
pass through. These are usually added to
give pearly shine, which offers no
improved cleansing. It provides only
optical effect.
• Eg: Spermaceti, Alkanolamides of higher
fatty acids, propylene glycol, Mg, Ca and
Zn salts of stearic acid etc
 Formulation Ingredients, contd…
Conditioners
• The conditioner functions to impart manageability, gloss, and
antistatic properties to the hair. These are usually fatty
alcohols, fatty esters, vegetable oils, mineral oils, or
humectants. Commonly used conditioning substances include
hydrolyzed animal protein, glycerin, dimethicone, simethicone,
polyvinylpyrrolidone, propylene glycol etc.
• Protein-derived substances are popular conditioners for
damaged hair, as they can temporarily mend split ends. Split
ends arise when the protective cuticle has been lost from the
distal hair shaft and the exposed cortex splits. The protein-
derived substances holds the cortex fragments together until
the next shampooing occurs.
Conditioners

22
Formulation Ingredients, contd…
Anti-dandruff Agents

• Medicated shampoos contain small amount of

these actives, which are in contact with the
scalp for only a short time. In order to be
effective the active ingredient must work in the
oil-water environment of the scalp and must be
readily substantive to the scalp for continuing
activity.
• Ex: Selenium sulfide, zinc pyrithone, salicylic
acid.
Formulation Ingredients, contd…
Perfumes

Shampoos include perfumes that are

mostly concentrated.

Example: Fruit fragrance

Formulation Ingredients, contd…
Colors

Used to impart color, different colors are

used.
Formulation Ingredients, contd…
Preservatives

Shampoo formula containing water has the

potential to be contaminated by pathogens.
For this reason it is essential to include
preservatives among shampoo ingredients,
to prevent the growth of molds.
Preservatives usually comprise only 0.1 –
0.5% of the formulation.
 Manufacturing Procedure

• Some agents are waxy solids at ambient

temperature and require melting in a
drum oven or similar before use.
• Demineralised water is most commonly
used in order to minimize contamination
of the product.
• No further processing is required after
blending, and the product may be packed
off directly from the mixing vessel.
 Quality Control

Foam Stability: Cylinder shake method is

used for determining foaming ability. 50ml
of the 1% shampoo solution is put in
250ml graduated cylinder, cover the
cylinder with hand and shake for 10 times.
The total volumes of the foam contents
after 1 minute shaking is recorded. The
foam volume is calculated. Foam should
retain for atleast 5mins.
Foam Stability = V2-V1
Quality Control, contd…
Wetting Action

Canvas disk is used to determine wetting

action. It is one inch in diameter. It floats
on the surface of a solution. The time
required for it to sink is measured
accurately.
Quality Control, contd…
Dirt Dispersion

Put two drops of shampoo in a large test

tube. Add 10ml dirt water and one drop of
Indian Ink. Close the Test tube and shake
for 5min.
Estimate the amount of Ink in the foam.
The dirt should stay in water portion.
Quality Control, contd…
Viscosity Determination
• Brookefield Viscometer is used to determine viscosity
of shampoos. 100ml of shampoo is taken in a beaker
and spindle is dipped in it for about 5min and then
reading is taken.
• Ostwald viscometer may be used for thinner shampoos.
Quality Control, contd…
pH Determination
• Mix 1gram of shampoo with 9ml of water
and determine the pH using pH meter at
27o Celsius.
• pH paper may be used to determine pH.
Quality Control, contd…
Skin Irritability Test

Draize test is performed in albino rabbits.

A set of six rabbits are used for testing each
material. Shampoos should be tested only
for a short duration, for not more than
4hours. These preparations are diluted
between concentrations of 8 to 10%.
You need lather to
know it's really
working.
IS IT A MYTH ??
You need lather to know it's really working, contd…

Facts about usage of shampoos

Foaming occurs when surfactant molecules

in the shampoo mix with air and create tons
of tiny bubbles. Ideally, while shampooing
hair, head should have only enough lather to
lubricate the hair and scalp.

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After a while, your hair
gets used to your
shampoo. That's why
you need to switch to a
new brand occasionally.
IS IT A MYTH ??
After a while, your hair gets used to your shampoo , contd…

Facts about usage of shampoos

MYTH.
Hair shaft is a dead structure. So it can't get used
to anything. It's just perception of how your hair
responds to a new formula.

The same shampoo used on the same hair under

the same conditions produces the same results. If
you are using the right shampoo for your hair
texture, you will get the same great results.

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 CROWNING GLORY OF
BEAUTIFUL HAIR IS
DEPENDENT UPON USING
A PARTICULAR HAIR
CLEANSING PREPARATION
IS IT A MYTH ??
Crowning glory of beautiful hair is dependent upon using a particular hair
cleansing preparation, contd…

Facts about usage of shampoos

• Hair shaft consists of three layers, namely cuticle,
cortex and medulla. Cuticle the outermost layer is
made up of 7-10 layers of hard keratin. The Cortex,
made up of hard keratin, constitutes approx 80%
of hairs total mass. It is a complicated structure of
parallel twisted fibre (polypeptide chains); the
appearance is similar to a rope, , hydrogen and di-
sulphide bond. The medulla is found in the center
of the hair shaft. Not every hair has a medulla.
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Crowning glory of beautiful hair is dependent upon using a particular hair
cleansing preparation, contd…

Facts about usage of shampoos

• The hair follicle is a pocket in the skin from where the hair
grows. The follicle grows through the epidermis and into
the dermis. There are three main parts of the follicle:
Papilla, The Germinal Matrix and The Hair Bulb.
• The papilla is found at the bottom of the follicle in the
dermis. This is where the blood capillaries pass nutrients
(food) and oxygen into the cells of the germinal matrix.
New cells start the process of keratinization at hair bulb.
• Thus, hair shaft is a dead structure. it gets nutrition from
the dermis. Hair cleansing preparations helps to make
hairs look better but does not provide nutrition.

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 Frequent
shampooing dries
your hair.
IS IT A MYTH ??
Frequent shampooing dries your hair, contd…

Facts about usage of shampoos

It is quite the contrary! Shampooing, if done
correctly and with the right products,
actually remoisturizes. The natural oils
produced by your scalp simply sit on top of
your hair shaft and do not penetrate it. It’s
moisture (i.e water) that does this, and also
a well formulated conditioner.

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Washing every day
can be bad for your
hair.
IS IT A MYTH ??
Washing every day can be bad for your hair, contd…

Facts about usage of shampoos

MOSTLY MYTH. If you have oily hair, it's fine to

wash every day--but even oily types should use a
gentle formula (one with moisturizing ingredients,
like silicones, shea butter, or panthenol). People with
coarse or dry hair might want to be more
conservative and wash every other day. No matter
what kind of hair you have, as long as you stay away
from harsh formulas that strip natural oils and treat
your strands with conditioner, regular shampooing
won't do any harm.

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 Frequent
shampooing makes
hair oilier.
IS IT A MYTH ??
Frequent shampooing makes hair oilier, contd…

Facts about usage of shampoos

• Myth.
• Clean clothes show dirt immediately.
Similarly, clean hair shows grease faster
than hair that is already oily. It is a matter of
individual perception. Things that actually
can increase oil production are hormones
and stress.

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 Frequent
shampooing makes
hair fall out.
IS IT A MYTH ??
Frequent shampooing makes hair fall out, contd…

Facts about usage of shampoos

• No. It is natural to lose up to 100 hairs a day and a
percentage of this comes out when you shampoo. The
act of shampooing simply dislodges hairs that have
already become detached from the follicle’s base are
ready to come out.

• However, on a day you don't shampoo, while some of

those strands will come out when you brush and style,
some of them will also remain sitting loosely in the hair
follicle. This means that the more days you leave
between shampooing, the more you will see in the drain.

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 References
1. Balsam, S.M., Gershon, S.D., Rieger, M.M., Sagarin, E., and Strianse, S.J.: COSMETICS–
Science and Technology, 2nd edition, Vol-2, John Wiley India, New Delhi, 2008
2. Barel, A.O., Paye, M., and Maibach, H.I.: Handbook of Cosmetic Science and
Technology, 3rd Edition, Informa Healthcare, New York.
3. Sharma, P.P.: COSMETICS - Formulation, Manufacturing and Quality Control, 4th
Edition, Vandana Publishers Pvt. Ltd., New Delhi, March 1998.
4. Butler, H.: POUCHER’S – Perfumes, Cosmetics & Soaps, 10th Edition, Springer,
Cockermouth, Cumbria, USA, 2000.
5. Salador, A., and Chisvert, A.: Analysis of cosmetic products, Elsevier, New York, 2006.
6. Ross, J., and Miles, G.D.: An application for comparison of foaming properties of
soaps and detergents, Oil and Soap, 1941.
7. Mittal,: A Handbook of Cosmetics
8. Fredell, W.G., and Powers, D.H.: Factors attributing to the performance of shampoos
and to consumer acceptance, Proc. Sci. Sec., 1955.
9. Rajkumar, K. J., Invitro evaluation of shampoos.
10. www.cosmeticdatabase.com
 Gitika Arora Dhingra
NCRD’s Sterling Institute of Pharmacy, Nerul, Navi Mumbai
E-mail: gitika.dh@gmail.com
 ANIONIC SURFACTANTS
CLASS EXAMPLE COMMENT
Alkyl benzene Sodium dodecyl benzene Tend to yield an “airy” or low density foam
sulfonates sulfonate and often are drying to the hair
Primary alkyl sulfates Lauric acid, stearic acid and Good lathering effect in hard water, free from
their salts rancidity, easy to wash.
Secondary alcohol Sodium sec-lauryl sulfate Low cost, dispersing and emulsifying action,
sulfates dissapointing as detergets and shampoo
components
Alkyl benzene Triton X200 Stable in acid or alkaline solution, excellent
polyoxyethylene emulsifier, detergent and wetting agent;
sulfonates extremely stable at pH of skin

Sulfated Lauric monoglyceride Stable in hard water

monoglycerides ammonium sulfate
Alkyl ether sulfates Derivatives of lauryl alcohol Good cleansers, act as solvents for non polar
ether with PEG additives
Sarcosines Lauroyl and cocoyl Excellent foaming and conditioning action
sarcosines
Sulfosuccinates Aerosol OT Less irritating to skin and eye (baby shampoo)
Maypon Protalbinic and lysalbinic Hydrolysation product of proteins with fatty
acid derivatives (maypon 4C) acid chlorides in presence of alkali
 NON-IONIC SURFACTANTS
CLASS EXAMPLE COMMENTS
Fatty acid Lauric monoethanolamide Improves solubility of SLS
alkanolamides (should Stearic ethanolamide Pearlescent thickener
not be used > 15%)
Oleic ethanolamides Hair conditioning agents
Polyalkoxylated Ethoxylated fatty alcohols Stable in wide range of pH; stabilizing
derivatives emulsifying and opacifying properties
Block polymers (pluronics) Good rinsability, can be used in high %
Sorbitol esters (TWEENS) Solubilizers and emulsifiers, used in baby
shampoos
Amine oxides Coconut and dodecyl Foam booster and anti-static agents
dimethyl amine oxides
AMPHOTERIC SURFACTANTS
N-alkyl aminoacids β – aminoacid derivatives Foaming agents
Aspargine derivatives Compatible with both anionic and
cationic surfactants
Betains Amido betains High foaming properties, mild.
Alkyl imidazoline MIRANOLTM Baby shampoos
 FORMULATIONS
POWDER SHAMPOO LOTION SHAMPOO
Henna powder 5% TLS 35%
Soap powder 50% Glyceryl monostearate 2%
Sodium carbonate 22.5% Magnesium stearate 1%
Potassium carbonate 7.5% Water Upto 100%
Borax 15% Color q.s
Perfume q.S Perfume, preservatives q.s

LIQUID SHAMPOO
SLS 40%
NaCl (to desired viscosity) 2-4%
Water Upto 100%
Perfume, color, preservatives q.s
 FORMULATIONS
CREAM SHAMPOO AEROSOL SHAMPOO
SLS 38% TLS 60%
Cetyl alcohol 7% Coconut diethanolamide 2%
Water Upto 100% Water Upto 90%
Color, perfume q.S Propellent 10%
Preservative q.s Color, perfume, preservative q,.s

JELLY SHAMPOOS
Alkyl dimethyl benzalkonium chloride 15%
TLS (40%) 28%
Coconut ditethanolamide 7%
HPMC 1%
Water Upto 100%
Color, perfume, preservative q.s
 FORMULATIONS
CONDITIONING SHAMPOOS BABY SHAMPOO
Steryl dimethyl benzyl 5.5%
Magnesium lauryl sulfate (27.5%) 11%
ammonium chloride
Ethylene glycol 2% Cocamidopropyl betaine (30%) 5%
monostearate
Cetyl alcohol 2.5% Polysorbate 20 1%
Water Upto 100% PEG 600 3.5%
Color, perfume, preservative q.s
Perfume q.S
TWO LAYER SHAMPOO
Preservative q.S
SLS 27%
Citric acid To pH 6
Cocamidopropylamine oxide 5%

Lauramine DEA 1% Color q.S

Lactic acid (50%) 1% Water (deionised); Aqua (INCI) To 100%

Formaldehyde 0.1%
 FORMULATIONS

ANTI-DANDRUFF SHAMPOO ANTI-DANDRUFF SHAMPOO

Thymol 0.05% Selenium sulfide 2.5%
Menthol 0.1%
Bentonite 5%
Camphor 0.1%
SLS paste 35%
TLS 55%
Water upto 100 Water upto 100
Color, perfume, preservative q.s Color, perfume, preservative q.s
 FORMULATION
HERBAL SHAMPOO
Natural essential oil blend 0.5%
Cyamopsis tetragonoloba (Guar Gum) 1%
Camellia sinensis (Green Tea) extract 2%
Glycerin 1%
Hydrolysed wheat protein 2.5%
Salvia officinalis (Sage) leaf extract 1.5%
Salvia officinalis (Sage) 1.5%
Glyceryl oleate 1%
Polysorbate 20 0.5%
Potassium sorbate 5%
Aloe barbadensis (Aloe vera) extract 0.5%
Arctium minus (Burdock) root extract 0.5%
Disodium coco-glucoside sulfosuccinate 0.5%
Preservatives q.s.
Water Upto 100%