USP Cosmetics lab Questions

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UNIT V
FORMULATION &
EVALUATION OF SHAMPOO
V.MANIMARAN
LECTURER
DEPARTMENT OF PHARMACEUTICS
SRM COLLEGE OF PHARMACY
CONTENTS
1. Introduction
2. Types of Shampoos
3. Product Ingredients
4. Formulation
5. Evaluation of Shampoos
6. References
Introduction
• Definition: 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.
• Requirements of a Shampoo:
1. It should effectively and completely remove dust or soil,
excessive sebum or other fatty substances and loose corneal
cells from the hair.
2. It should produce a good amount of foam to satisfy the
psychological requirements of the user.
3. It should be easily removed on rinsing with water.
4. It should leave the hair non‐dry, soft, lustrous with good
manageability and minimum fly away.
5. It should impart a pleasant fragnance to the hair.
6. It should not cause any side‐effects / irritation to skin or eye.
7. It should not make the hand rough and chapped.
Types of
Shampoo
Shampoos are of the following types:
¾ Powder Shampoo
¾ Liquid Shampoo
¾ Lotion Shampoo
¾ Cream Shampoo
¾ Jelly Shampoo
¾ Aerosol Shampoo
¾ Specialized Shampoo
• Conditioning Shampoo
• Anti‐ dandruff Shampoo
• Baby Shampoo
• Two Layer Shampoo
PRODUCT INGREDIENTS
• Surfactants are the main component of shampoo. Mainly anionic
surfactants are used.
• The raw materials used in the manufacture of shampoos are:
1. Principal surfactants: Provide detergency and foam.
2. Secondary surfactants: Improve detergency, foam and hair
condition.
3. Other additives.
CLEANSING ACTION OF SHAMPOO
A surfactant consists of two part‐ one hydrophilic (water loving)
while the other is hydrophobic in nature.
Surfactants
¾ 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.
¾ Non‐ionic surfactants have good cleansing properties
but do not have sufficient foaming power.
¾ Cationic surfactants are toxic and are hence not used.
However, they may be used in low concentration in
hair conditioners.
¾ Ampholytics, being expensive, are generally not used.
However, they are mainly used as secondary
surfactants and good hairconditioners.
ANIONIC SURFACTANTS
CLASS
EXAMPLE
COMMENT
Alkyl benzene
sulfonates
Sodium dodecyl benzene
sulfonate
Tend to yield an “airy” or low density foam
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
sulfates
Sodium sec‐lauryl sulfate
Low cost, dispersing and emulsifying action,
dissapointing as detergets and shampoo
components
Alkyl benzene
polyoxyethylene
sulfonates
Triton X200
Stable in acid or alkaline solution, excellent
emulsifier, detergent and wetting agent;
extremely stable at pH of skin
Sulfated
monoglycerides
Lauric monoglyceride
ammonium sulfate
Stable in hard water
Alkyl ether sulfates
Derivatives of lauryl alcohol
ether with PEG
Good cleansers, act as solvents for non polar
additives
Sarcosines
Lauroyl and cocoyl
sarcosines
Excellent foaming and conditioning action
Sulfosuccinates
Aerosol OT
Less irritating to skin and eye (baby shampoo)
Maypon
Protalbinic and lysalbinic
acid derivatives (maypon 4C)
Hydrolysation product of proteins with fatty
acid chlorides in presence of alkali
NON‐IONIC SURFACTANTS
CLASS
EXAMPLE
Fatty acid
alkanolamides (should
not be used > 15%)
Lauric monoethanolamide
Improves solubility of SLS
Stearic ethanolamide
Pearlescent thickener
Oleic ethanolamides
Hair conditioning agents
Polyalkoxylated
derivatives
Ethoxylated fatty alcohols
Stable in wide range of pH; stabilizing
emulsifying and opacifying properties
Block polymers (pluronics)
Good rinsability, can be used in high %
Sorbitol esters (TWEENS)
Solubilizers and emulsifiers, used in baby
shampoos
Coconut and dodecyl
dimethyl amine oxides
Foam booster and anti‐static agents
Amine oxides
COMMENTS
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
ADDITIVES
¾
¾
¾
Conditioning agents: Lanolin, mineral oil, herbal extracts, egg
derivatives.
Foam builders: Lauroyl monoethanolamide, sarcosinates
Viscosity modifiers :
™
™
™
™
™
Electrolytes – NH4Cl, NaCl
Natural gums – Gum Karaya, tragacanth, alginates
Cellulose derivatives – Hydroxy ethyl cellulose, methyl cellulose
Carboxy vinyl polymers – Carbopol 934
Others – PVP, phosphate esters.
¾ Sequestering agents : EDTA
¾ Opacifying agents : Alkanolamides of higher fatty acids, propylene
glycol, Mg, Ca and Zn salts of stearic acid, spermaceti, etc.
¾ Clarifying agents :
™ Solubilizing alcohols – ethanol, isopropanol
™ Phosphates –
™ Non‐ionic solubilizers – polyethoxyated alcohols and esters.
ADDITIVES
¾ Perfumes : Herbal, fruity or floral fragnances.
¾ Preservatives : Methyl and propyl paraben,
formaldehyde (most effective).
¾ Anti‐dandruff agents: The 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.
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
Steryl dimethyl benzyl
ammonium chloride
5.5%
Ethylene glycol
monostearate
BABY SHAMPOO
Magnesium lauryl sulfate (27.5%)
11%
2%
Cocamidopropyl betaine (30%)
5%
Cetyl alcohol
2.5%
Polysorbate 20
1%
Water
Upto 100%
PEG 600
3.5%
Perfume
q.S
Preservative
q.S
Citric acid
To pH 6
Color, perfume, preservative q.s
TWO LAYER SHAMPOO
SLS
27%
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
Thymol
0.05%
Menthol
0.1%
Camphor
0.1%
TLS
55%
Water
Color, perfume, preservative
ANTI‐DANDRUFF SHAMPOO
Selenium sulfide
2.5%
Bentonite
5%
SLS paste
35%
upto 100
Water
upto 100
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%
Evaluation of Shampoos
ƒ Performance characteristics
9 Foam and foam stability
9 Detergency and cleaning action
¾ Effect of water hardness
¾ Surface Tension and wetting
¾ Surfactant content and analysis
9 Rinsing
9 Conditioning action
¾ Softness
¾ Luster
¾ Lubricity
¾ Body, texture and set retention
¾ Irritation and toxicity
¾ Dandruff control
9 Microbiological assay
9 Eye irritancy test
ƒProduct characteristics
9Fragnance
9Colour
9Consistency
9Package
1.
•
•
•
2.
•
•
•
•
Foam and foam stability:
The Ross‐Miles foam column test is accepted. 200 ml of surfactant
solution is dropped into a glass column containing 50ml of the same
solution. The height of the foam generated is measured immediately
and again after a specified time interval, and is considered proportional
to the volume.
Barnett and Powers developed a latherometer to measure the effect of
variables such as water hardness, type of soil and quantity of soil on
foam speed, volume and stability.
Fredell and Read titrated actual standard oiled heads of hair with
additive increments of shampoo until a persistent lather end point
appeared.
Detergency and cleaning action:
Cleansing power is evaluated by the method of Barnet and Powers
5gm sample of soiled human hair is placed at 35°c in 200 cc of water
containing of 1 gm of shampoo.
The flask is shaken 50 times a minute for 4 minutes. Then washed once
again with sufficient amount of water, then after filter the hair dried
and weighed.
The amount of soil is removed under these condition is calculated.
3. Wetting Action:
• Canvas disk sinking test: A mount veron cotton duck # 6 canvas disk 1
inch in diameter, is floated on the surface of a solution, and the time
required for it to sink is measured accurately.
4. Rinsing:
• Skilled beauticians are employed to make comparisons on the
performance of several shampoos.
5. Conditioning Action:
• Conditioning action is a difficult property to assess. This is because it is
basically dependent on subjective appraisal.
• No method has been published for measuring conditioning action.
• The degree of conditioning given to hair is ultimately judged by
shampoo user who is making the evaluation on the basis of past
experience and present expectations.
6. Microbiological assay:
‰ PREPARATION OF PRE‐INOCULUM Take the loopful culture of
staphylococcus aureus (ATCC6532) aseptically and transfer to
sterilized and cooled 100 ml SCDM (broth).
• Mix well. Incubate the broth at 37oC for 24 hrs.
‰ PREPARATION OF MEDIA Soya bean casein digests medium, soya
bean casein digest agar and nutrient agar.
‰ PREPARATION OF POUR PLATES Sterilized SCD agar (100 ml) is
cooled to 40°C and mixed with 5 ml of 24 hrs old pre inoculated
culture.
• This is immediately poured in plates (340 ml each) and allows to
set.
‰ MAKING THE WELLS ON AGAR PLATES The wells are dig on agar
plates with sterilised well digger aseptically.
• Take 100µml of each sample, add to well aseptically. Incubate the
plates at 37oC for 24 hrs to 48 hrs.
• Observe the effectiveness of sample on culture growing on the agar
plate and we can see the effectiveness of sample in the form of
zone of inhibition around each well containing different sample.
7. Evaluation of eye irritancy:
•
•
•
•
•
•
The test calls for dropping 0.1 ml of liquid shampoo in the
conjunctiva sac of one eye of the rabbit , the other eye serving as
control.
In the case of the first three animals, the treated eye remains
unwashed. Since washing the eye may or may not alleviate
symptoms of injury.
The six remaining animals are divided into two equal groups.
In the first of these groups eyes instilled with the substances are
washed with 20 ml of lukewarm water two seconds after
treatment and in the second group after instillation.
Readings are then made at 24, 48 and 72 hr and again four and
seven days after treatment.
If the lesions have not cleared up in seven days the test material is
considered as severe irritant.
8. Viscosity:
•
•
Viscosity of the liquid shampoo is determined using a Brookefield
viscometer
100 mL of the shampoo is taken in a beaker and the spindle is
dipped in it for about 5 min and then the reading is taken.
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
BUENAFE, CHAVEZ, CRISOSTOMO, DELA VEGA, LUGO | 3B-PH
[3] SHAMPOO
SHAMPOO
 From a Hindi word “champo”, meaning “to press or to
massage”
 The main benefit if shampoo is the removal of dirt from the
hair.
 Hair care product designed to clean the scalp skin along
with its hairs.
o
o

Before Shampooing



o
o
In formulation a shampoo or other hair care products, it must be
assured to use safe ingredients. Because there are tendencies in
manufacturing companies due to their wants to market the product on
a competitive price, they tend to use cheaper ingredients. Not to
generalize, but some cheap ingredients are of low quality.
Generally, shampoo do not cause skin irritation because it only has a
short duration of contact on the skin. But there are some consumers that
have sensitive skin and develops irritation in some shampoo.
The main problem in shampoos is ocular irritation instead if skin
irritation.
Its use should result to
Soft
Manageable; a
Lustrous form hair
SHAMPOO FORMS
CLEAR LIQUID SHAMPOO
 Liquid soap
o
o


Shampoo contains surfactants. The Surfactants looks like the phospholipid unit of
the plasma membrane. There’s a hydrophilic head and a hydrophobic tail. The
hydrophobic tail attaches to the oil/dirt present in our hair. If the surfactants
already entrapped the oil/dirt it looks like the micelle in the picture above, the
hydrophilic head is on the external part. When you rinse it, since the hydrophilic
head are in external part, it will now join the water. Surfactants are the one
responsible for the cleaning action of shampoos
Before
Shampooing
Mode of
Action
Rinse
o


lathering means building of foam or bubbles
3. better rinsability.
Usually based on potassium soap o because of its greater
solubility
o
o
MECHANISM OF COSMETIC ACTION ON SHAMPOO
Liquid shampoo or liquid soap
An example is the Johnson’s baby shampoo or other pediatric shampoo.
The clear liquid gives a psychological impression that the shampoo/
liquid soap is mild
Most popular because of
1. the ease of application
2. rapidity of lathering
o
o
o
o
After Shampooing
The left side picture depicts a hair with oil and dirt. While the right side is the
cleansed hair after shampooing
There are hair products that take longer time to be removed in the hair so it
needs shampooing for 2 to 3 times before its total elimination. These products
usually have long lasting effect such as the waxes.
Upon Shampooing, is our goal to remove all the oil in our hair/scalp?
o
The answer is no. The oil is for the moisturizing. If all he oil is removed,
the hair will be dry and will look dull.
It should not affect adversely the hair, scalp and the health
of the user.
o

Sample of dirt are: sweat, sebum, dead skin, environmental pollutants.
These dirts are not soluble in water. Therefore, washing the hair with
simply with water would not be enough to really clean the hair. Use
shampoo in order to completely remove all those dirts because shampoo
contains ingredients that are able to remove those oily, non-water
soluble particles. Particularly, the ingredient responsible for that is the
surfactants. Because shampoo is actually as surfactant-based cosmetic
product.
Other hair care products:

Conditioner

Hair mask (usually embedded with vitamins for the hair),

Gel is a hair setting product not a hair cosmetic product

Hair oil – adds volume to the hair. An example is the (VCO)Virgin
coconut oil, which induces hair growth

Leave-in conditioner
The higher the solubility, the easier it is to rinse
Potassium hydroxide is used usually in making soft soap or liquid soap.
Potassium is used since it is usually used in making liquid soap or soft
soap.
For hard soap, Sodium Hydroxide is used.
Stable, easily colored, perfumed
Uses SLS, SLES, foam builders (CDA)
o
o
SLS, SLES are surfactants
CDA – Cocodiethylamine
LOTION SHAMPOO

Has a thicker viscosity or thicker texture compared to a clear liquid shampoo
Parts:
1. Active Ingredient
o
Skin
Oil and dirt
are attached
to the skin
and hair
Skin
The
surfactant
lowers the
surface
tension of
water
Skin
The
surfactant
creates
micelles
around the
dirt and oil
that are
removed
from the skin
and hair
Skin
The micelles
with the oil,
dirt, and
surfactant
are
eliminated
with water
during rinse
2.
Used if you want to add an active ingredient such as for anti-dandruff
effect
Opacifier- pearly look to shampoo
o
Gives off the shining effect of the shampoo. Addition of opacifier gives
a psychological impression that the shining effect ca be transferred to
your hair
CREAM SHAMPOO





The most common type of shampoo.
The shampoo we used on day to day basis are usually cream shampoos
Opaque and viscous
Mixture of SLS and soap
Makes the shampoo viscous.
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BUENAFE, CHAVEZ, CRISOSTOMO, DELA VEGA, LUGO | 3B-PH
SHAMPOO COMPONENTS

This is the most common component of shampoos, but since we have a lot of variety
of shampoo, the components also vary a lot depending on the claim of the shampoo.
COMPOUND FOR SPECIALIZED CAPABILITIES
 Minimizing eye sting; should have low
(sulfosuccinate)
o
irritancy
Sulfosuccinate is usually found in Johnson’s Baby Shampoo or shampoos
for the pediatric population. This is because sulfosuccinate has low
irritancy and therefore minimize the tendency of eye irritation. Hence,
the claim of Johnson’s Baby Shampoo of “No More Tears” because the
surfactant used had low irritancy.
CONTROLLING DANDRUFF
 Zinc pyrithione (ZPT), selenium sulfide, ketoconazole
o
o
o
o
o
o
o
Zinc pyrithione is usually found in Head n’ Shoulders, which has a claim
of “We are the world’s Number #1 anti-dandruff shampoo”.
As mentioned, selenium sulfide is the most common anti-dandruff active
ingredient (API).
Another is ketoconazole, under the brand name Nizoral, but it is not
used as often anymore due to selenium sulfide. Unlike before, when
selenium sulfide was not marketed in the Philippines.
Aside from Head n’ Shoulders, we have Clear Anti-Dandruff Scalp Care
Shampoo and it also contains different ingredients for its anti-dandruff
effect.
There are shampoos that are 2-in-1(shampoo + conditioner). A
common example is Palmolive Naturals. If we look at the ingredients,
it has surfactants and ingredients with conditioning effect. Also, taking
note that their name has ‘Naturals’, this is because their products contain
botanical extracts such as Aloe Vera. Before, Palmolive was known to
formulate the world’s most bestselling soaps due to their moisturizing
effect – the moisturizing effect comes from the key ingredients, palm
oil and olive oil; hence the name “Palmolive’’.
There are also those with conditioning effects such as Cream Silk Triple
Keratin Structure. Keratin is a basic protein that makes up our hair, skin,
and nails. So it is better if products have keratin.
SunSilk is a shampoo that contains vitamins such as Biotin, a watersoluble vitamin which helps in keratin infrastructure. It also contains Aloe
Vera
IMPARTING APPEALING FRAGRANCE
 Gain a more favorable fragrance acceptance

As mentioned, aesthetic appeal is important in cosmetic products. An
example is Rejoice which is a fragrant-rich shampoo.
But if the ingredient used is SLS, then it is directly correlated that more lather
means a better cleansing effect. However, not all products have SLS as their
foam builder.
CONDITIONING AGENT

Moisturizes and lubricates the hair for better slip and
smoothness

E.g. lanolin, glycerol, propylene glycol, isopropyl myristate


Primarily, shampoos are used as cleansing agent but if the hair is too clean,
if all oil was removed, if the a high-concentration/level surfactant was used,
then a conditioning agent is needed to moisturize and lubricate the hair.
There are people who do not want to use or like to use conditioners because
they are hard to rinse; however, this is normal because the effect of
conditioning agent is that they leave a film on the surface of our hair or scalp
which will improve the slip and smoothness of the hair.
OPACIFYING AGENT (PACIFIERS)

Important for cream and lotion shampoo

E.g. higher alcohol (stearyl and cetyl), higher acids (behenic
acid)

This agent plays an aesthetic role by providing a unique pearly and
shimmering effect in the shampoo
CLARIFYING AGENTS

solubilizing agents help maintain shampoo’s clarity over a
wide range of temperature.

They should be checked for possible eye irritation

E.g. butyl alcohol, isopropyl alcohol, propylene glycol,
terpineol, diethylene glycol, diethyl alcohol


Induces the clarity of the shampoo, especially if you’re formulating a clear
liquid shampoo
During R&D, when formulating a shampoo, we need to remember that we
should optimize the correct amount of agents because, for instance, too much
clarifying agent (to maintain clarity of the shampoo) may compromise the
pathological safety of the product. This is because clarifying agents may
cause eye irritation since most of the examples are alcohol.
SEQUESTERING/CHELATING AGENTS

Prevents lime soap formation by:
1.
Formation of insoluble calcium or magnesium salts when
mixed with hard water
2.
Precipitation of lime soap film on the hair when the
shampoo is rinsed with hard water
o
SURFACTANTS
 Detergent shampoo
 Washes the hair





This is the ingredient responsible for the cleansing effect of shampoo. We
have different types of surfactants – anionic, cationic, non-ionic, and
amphoteric.
Anionic surfactants – most commonly used because of its good cleansing
effect (E.g. SLS, SLES, triethanolamine lauryl sulphate)
Cationic surfactants – not as popular as anionic since they do not foam/lather
very well; but it is used for shampoos that require soft and manageable
effects of the hair. These are included in shampoos used after dyeing your
hair due to its dry state. Salons usually recommended ‘non-sulphate
shampoos’ since they contain cationic surfactants.
Amphoteric surfactants – responsible for the non-irritating effect. Usually,
anionic surfactants are used in combination with amphoteric surfactants since
anionics have the foam stabilizing effect. But for non-irritating formulations,
amphoteric has a larger amount than anionics.
Non-ionic surfactants – are very mild but they are usually in combination with
anionic surfactants.
FOAM BUILDERS

Foam stabilizer

Increases quality, volume, and stability of lather

E.g. SLS (sodium lauryl sulphate), CDA

Some consumers like their shampoo to have better lathering. Since they expect
that more lather means a better cleaning effect. Although, we cannot directly
correlate the foaming effect/property of the shampoo to its cleansing power
because the ingredients responsible for each are different.
o
o
Lime soaps are insoluble salts of calcium and magnesium that is
formed when they interact with hard water
Lime soaps can be seen in bathrooms, they are usually the white
precipitate found on tiles. In shampoo formulations, sequestering
agents or chelating agents are added to prevent the formation of
lime soaps.
An example is EDTA
ANTIDANDRUFF

Addition of selenium dioxide and zinc pyrithione
THICKENING AGENT

Increases and controls viscosity

E.g. synthetic gums, inorganic salts, longer-chain acids,
longer-chain alcohols and amides


Responsible for the rheological property of the shampoo
If the shampoo is not viscous or too watery, you won’t be able to use it
properly; but if it is too viscous, it’ll be hard to get from the packaging, so
we have to optimize the thickening or the viscosity of the formulation during
R&D
PRESERVATIVE

Formaldehyde, Ethanol, paraben
o
o
Formaldehyde is not used as a preservative anymore because of its
carcinogenic effect. Similarly, paraben is also not used as often
anymore due to its carcinogenic effect.
Usual preservative used today are ethanol if applicable and sodium
benzoate.
STABILITY ADDITIVES

Antioxidant, sunscreen, suspending agents, pH control drugs
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BUENAFE, CHAVEZ, CRISOSTOMO, DELA VEGA, LUGO | 3B-PH
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Some formulations may contain ingredients sensitive to oxidation, so
antioxidants are added.
Too low or too high pH level could cause irritation. So the ideal pH range for
shampoo is 6.5 – 8. 5
SUPPLEMENTAL VIDEO ON SHAMPOO FORMULATION
COSMETIC ADDITIVES

Perfume, dye, tints, pearlescent
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In shampoos, or cosmetics in general, your perfume or dye or the color of the
formulation should complement each other
Fragrance and color or dye has a psychological impression to consumers. For
example, if the shampoo is for men, the usual colors are blue, green with
scents such as menthol or cooling aroma. For women, the usual colors are pink
and white with fragrance such as fruity scents.
QUALITY CONTROL OF SHAMPOOS
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Pass the “product use test”
Should meet cleansing, rinsing, conditioning, and most
importantly:
o The safety criteria for the product
o Aesthetic characteristics

Making shampoo includes 3 different surfactants, a thickener, a moisturizer,
and a preservative.


Start with the water phase at 56%.
The first ingredient is a non-ionic surfactant called sulfosuccinate. It has good
degreasing power but still mild, so add 15%.
The next ingredient is coco betaine, which is a coconut-based surfactant.
Amphoteric type has good foaming and a bit of thickening property. We add
15% as well.
The third surfactant is polyglucose, a non-ionic surfactant. It is a very mild
product so we’ll add just 5%.
The next ingredient is PEG-7 glyceryl cocoate. It is an emollient and
moisturizer (coconut-based) that will give moisture to the hair. We will add
2%.
Then we will need a conditioner so it will leave the hair slightly conditioned.
So we’ll use the Quarternium-31 which is a good detangler. We will add 4%.
In any preparation, three things should be considered – quality, efficacy, and
safety. In shampoos, the qualities to be considered are its spreadability and
extrudability. Extrudability is the power required to push something out of the
packaging. Is the product easily squeezed out of the package?
The foam property and foam stability, the efficacy of the preservative, pH
and viscosity should also be checked.
For the efficacy of the shampoo, the only thing needs to be tested, if
applicable, is the anti-dandruff claim.
Also, efficacy of preservative and anti-oxidants should be tested if they really
prevent or protect the product from microbial growth and chemical
degradation.
Lastly, for the safety of shampoo, the ocular irritation potential is tested.
SHAMPOO PREPARATION
Mix coconut diethanolamide (CDA) with
methyl paraben and propyl paraben

Add sodium laureth sulfate and mix for 5
minutes
add lanolin and mix for 5 minutes
add fragrance oil



add enough purified water to make 750
mL and add enough colorant
CDA is the foam builder mixed with the parabens or preservatives. Then SLS or the
surfactant is added and mixed for 5 minutes. Then add lanoline which is your
conditioning agent and mix for 5 minutes.
SHAMPOO FORMULATION INGREDIENTS USED IN THE
SUPPLEMENTAL VIDEO
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

Water 56%
Sulfosuccinate (surfactant) 15%
Coco Betaine (surfactant) 15%
Polyglucose (surfactant) 5%
PEG 7-Glyceryl Cocoate (emollient) 2%
Quaternium-31 (detangler) 4%
Glucose-T (thickener) 2%
Phenoxyethanol/Sorbic Acid (mild preservative blend) 1%
Fragrance

As you can see [refer to picture above], the shampoo is still very thin so we
will add a thickener called Glucose-T. Only 2% is needed so it will thicken
nicely. Then stir.
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BUENAFE, CHAVEZ, CRISOSTOMO, DELA VEGA, LUGO | 3B-PH

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
In the video, they used water (cosmetic vehicle) already instead of CDA and
paraben. This is because all the ingredients used in the video are in liquid
form.
But in our case, CDA from coconut oil is oil in nature while the paraben,
propylparaben, SLS, and lanolin are solid in nature (lanolin is semi-solid, SLS
and paraben is powder). We added all the solids in nature first to have a
better solubility. And then we add the fragrance then the water.
The manufacturing procedure actually depends on the ingredients used.
In manufacturing companies, liquid formulations are preferred to use closed
systems or closed container systems to prevent microbial growth and
contamination.
In our laboratory, we do not use the top loading balance. We will weigh or
measure the ingredients individually and then mix them together according to
the procedure.
END
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As you can see [refer to picture above], it is already starting to thicken. Once
the ingredients are mixed, we will add a preservative.
We will add a very effective preservative but a mild one called
phenoxyethanol/sorbic acid. We will add 1%. Again, mix the ingredients
well.

[Refer to picture above]. It is not whitish, but it will clear overnight.


It will look like the picture above. It has a really nice flow and it’s looks clear.
Next, test the pH to see if it is in a good pH range (skin friendly between pH
4.5-6). Dip a piece of pH indicator strip in the shampoo and compare it to
the scale.
The shampoo formulation is finished. But you may add your favorite scent
(e.g. mangosteen, peach and ginger, Coconut Lime Verbena, or Pineapple
Lilies). They can be added at the end and all you have to do is package it
and put a label on. Your hair shampoo is now finished.

NOTES FROM THE VIDEO:

Since our skin is slightly acidic according to some studies, it is beneficial that
the sample is near pH 4.5. However, the ideal would be pH 6.5-8.5 (which
we will base for the sake of the course) because if it is too acidic it can cause
irritation.
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