BP809ET: Cosmetic Science

By
Lekkala Lithin Kumar
12001462, A05
YDE05

Submitted to
Dr. Sheetu
 QUALITY CONTROL TESTS FOR HAIR SHAMPOOS
Cosmetics are defined as "articles with mild action on the human body, which are intended to
be applied to the human body through rubbing, sprinkling or other methods, aiming to clean,
beautify and increase the attractiveness, alter the appearance or to keep the skin or hair in
good condition hence a modern face powder is a blend of several constituents. Cosmetics are
products that are created for application on the body for the purpose of cleansing, beautifying
or altering appearance and enhancing attractive features. Cosmetics are substances used to
enhance the appearance or odour of the human body [1,2,3].

A shampoo is a preparation containing surfactant 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. Most shampoos
contain water, a detergent (cleaning agent), surfactant (lather making agent), salt, fragrance
(natural and artificial), preservative, and food colouring. With the exception of water and salt
(sodium chloride), different chemical compounds are used depending on the desired result of
the shampoo [4].

Dandruff is a chronic scalp condition that causes scaling, itching and redness of the scalp by
shedding epidermal cells. The cause of dandruff is a fungus called Malassezia restricta and
Malassezia globosa. Malassezia, formerly known as Pityrosporum, is a yeast that causes skin
and scalp infections. For the treatment of dandruff, hair care preparations typically contain
antifungal agents. Many of these products have side effects such as loss of hair, increased
scaling, itching, irritation, nausea, and headaches. Dandruff can be treated in two ways, using
herbal-based antidandruff shampoo and using chemical-based anti-dandruff shampoo. The
dandruff shampoo bar was developed to be effective in treating the problem [5]. The choice
of "active" depends on the regulatory requirements in the market to be served. Currently,
there are five ingredients approved for use in over-the-counter (OTC) anti-dandruff products
in the United States. Zinc pyrithione and selenium sulfide are the most popular activ e
ingredients, followed by salicylic acid, sulfur, and coal-tar solution. Except for coal tar and
salicylic acid, the other three ingredients are used as suspensions in shampoo formulation.
Many shampoos also contain vitamins and moisturizing alcohols to prevent too much of the
hair and scalp’s natural oils from being stripped away during cleansing. The purpose of
antidandruff agents is to reduce the formation of dandruff flakes [6].
Ideal characteristics of shampoo:

 Shampoo should effectively remove the dust and excess sebum from hair and scalp.
 Shampoo should effectively wash hair.
 Shampoo should be easily removed by rinsing with water. Shampoo should leave hair
non-dry, lustrous, and
 good manageability.
 Shampoo should not make hand rough
 Shampoo should not have any side effect and should not irritate skin and eye.
 Shampoo should spread easily and disperse easily overhead and hairs.
 Shampoo must develop dense and luxurious lather
 It should be effective in a small amount.
 Ease of combing of wet hair [19].

The shampoo classification, listing different types of products:

 Powder shampoo
 Liquid shampoo
 Lotion shampoo
 Solid gel shampoo
 Liquid herbal shampoo
 Solid cream shampoo
 Aerosol foam shampoo
 Specialized shampoo
 Conditioning shampoo
 Anti dandruff Shampoo
 Baby Shampoo [19].

Category Ingredients
Surfactants Alpha olefin sulfonate, sodium lauryl sulphate, ammonium lauryl
sulphate, and ammonium laureth sulphate
Thickeners Natural gums, cellulose derivatives, and electrolytes
Sequestering agents EDTA
Additives Foam stabilisers, polyacrylate-based lubricants for controlling
viscosity, and dispersants
Humectants Glycerine, sorbitol, glycerol, propylene glycol, and polyethylene
glycol
Moisturizers Alkanolamides, natural oils
Preservatives Parabens
UV absorbers Benzophenones
 Buffers Sodium citrate
Anti-dandruff Zinc pyrithione, ketoconazole, piroctoneolamine,
agents ciclopiroxolamine, and selenium disulfide
[8]

S.n
Shampoo Variant
o
1. Clinic Plus Health shampoo
2. Head & Shoulders Silky black
3. Sunsilk Teddy thick and long
4. Dove Damage therapy/Intense repair
5. Pantene Silky smooth care
6. Revlon Gentle cleansing, extra body flex
7. Garnier Fructis Long & strong
8. L’Oreal Paris Smooth & intense
9. Himalaya Herbals Protein
10. Lotus Herbals Kera veda
11. Jovees Honey & apple
12. Biotique Bio green apple
[20]
Quality Control:

Quality control is essentially a tool which enables to maintain product quality at desired level.
In other words it maintains value of a product. Quality control is an ongoing process. It is a
comparison with a standard whether a cosmetic product adheres to a certain criteria.
Standards consist of:

1. Formula: This gives precise statement of different ingredients which comprise the
product.
2. Operating Standards: This gives detail of manufacturing procedures, storage, filling
and packaging.
3. Raw material Specification: Giving all details of characteristics and limits of
deviations permissible.
4. Packaging material standards: It covers all components which go around the
product shape, size, colour and other aesthetics and acceptance criteria and limits.
5. Finished product standard: It covers all characteristics essential for proper
performance, durability and safety of product .
6. Testing methods: This covers tests procedures of all components [7].
Objectives of Quality Control Tests:

1. To establish standards of quality which are acceptable to consumers.

2. To ensure that the customers are provided with products which conform with the
standard specifications.
3. To locate and identify process faults and defects of products.
4. To ensure that defective items are not used.
5. Evaluation of quality standards of incoming material, product in actual manufacture
and of outgoing product.
6. Judging the conformity of the process to the established standards, and taking suitable
action when deviation is noted.
7. Evaluation of optimum quality obtainable under given conditions.
8. To improve quality and productivity by process control and experimentation.
9. To ensure that defective products are not passed to customer.
10. Developing quality consciousness both within and without the organization [7].

The quality control tests performed for shampoos are as follows:

 Physical
appearance/ pH
Stability Visual determination
studies inspection

Chemical Dirt
tests Dispersion

Percentage
Microbiological solid
contamination content

Quality Control tests Surface

Viscosity Tension
measurement

Cleaning
Ash content
action

Moisture Wetting
content Foaming Time
Loss on ability and
drying Foaming
index

1. Physical appearance/Visual inspection: The formulations were evaluated in terms

of their clarity, colour, odour and texture. The formulation's colour was tested against
a white background. The odour of the formulation was assessed by smelling it [9].
2. pH determination: The pH levels of the different shampoos tested in 1% and 10%
water solutions were evaluated using a pH meter (pH/ORP meter, HI 2211 Hanna
instrument, Michigan, USA) at a room temperature of 25 ± 2 °C, based on the work of
several Pauthors. Most shampoos are neutral or slightly acidic. Acidic solutions cause
the cuticle (outer layer) of the hair to shrink and lie flatter on the hair shaft. Basic
solutions cause the cuticle to swell and open up. Acidic solutions make the hair
smoother, while basic solutions make the hair frizzier [9,10].
Standard Value= Around pH 6.2 [26].
3. Dirt Dispersion: Two drops of shampoo were added in a large test tube contain 10 ml
of distilled water. One drop of India ink was added; the test tube was stoppered and
shakes it ten times. The amount of ink in the foam was estimated as None, Light,
Moderate, or Heavy. Shampoos that cause the ink to concentrate in the foam are
 considered poor quality. The dirt should stay in the water portion. Dirt that stays in the
foam will be difficult to rinse away. It will redeposit on the hair [11].
4. Determination of percentage solid content: A clean dry evaporating dish was
weighed and added 4 grams of shampoo to the evaporating dish. The dish and
shampoo were weighed. The exact weight of the shampoo was calculated only and put
the evaporating dish with shampoo was placed on the hot plate until the liquid portion
was evaporated. The weight of the shampoo only (solids) after drying was calculated.
If a shampoo has too many solids it will be hard to work into the hair or too hard to
wash out. If it doesn’t have enough, it will be too watery and wash away quickly.
A good shampoo will be between 20% – 30% solids [12].
5. Surface tension measurement: Surface tension measurements were carried out using
a solution of 10% shampoo diluted in distilled water at room temperature using a
dropper. The dropper was thoroughly cleaned using chronic acid and purified water
since surface tension is highly affected by grease or other lubricants. Surface tension
was calculated by the following equation:
R2= (W3-W1)n1/ (W2-W1)n2 * R1
where W1 is the weight of the empty beaker and W2 is weight of the beaker with
distilled water; W3 is the weight of the beaker with the shampoo solution; n1 is the
number of drops of distilled water and n2 is number of drops of the shampoo solution.
R1 is the surface tension of distilled water at room temperature while R2 is the
surface tension of the shampoo solution [13].
6. Cleaning action: 5 grams of wool yarn were placed in grease, after that it was placed
in 200 ml. of water containing 1 gram of shampoo in a flask. Temperature of water
was maintained at 350C. The flask was shaked for 4 minutes at the rate of 50 times a
minute. The solution was removed and .sample was taken out, dried and weighed. The
amount of grease removed was calculated by using the following equation:
DP = 100 (1-T/C)
In which, DP is the percentage of detergency power, C is the weight of sebum in the
control sample and T is the weight of sebum in the test sample [14].
7. Wetting time: Wetting time was measured using Drave’s test, wherein some kind of
weighed skein (velvet) was allowed to sink through a wetting solution in a 500-mL
graduated cylinder, and the time taken for sinking was considered as the wetting
efficiency(*pharmaceutical evaluation). The Filter paper 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 of 1% w/v and the stopwatch started. The time required for the disc
to begin to sink was measured acutely and noted as the wetting time.
Standard Value= 3 sec [9,15,26].
8. Foaming ability and Foam index: This can be determined by using cylinder shake
method. 1% of shampoo preparation (50 ml) transferred to 250 ml graduated cylinder
and should be covered with one hand and shaken Upton 10 minutes the total volume
of foam after 1 minute of shaking must be recorded.
Standard Value= 0.9 to 2.5 cm
One gram of shampoo was weighed accurately and transferred into 250 ml conical
flask containing 100 ml of boiling water. Then it is warmed gently for 30 minutes,
cooled and filtered and make up the volume to 100 ml in standard volumetric flask.
This extract is taken in 5 test tubes in a series of successive portion of 1, 2, 3, 4, 5 and
remaining volume is made up with water to 10 ml. Then the test tubes were shaken in
longwise motion for 15 seconds at speed of 2 frequencies / second. Then the tubes are
allowed to stand for 15 minutes. The height of the foam was measured.
Foaming index =1000/a [26]

9. Loss on drying: Loss on drying is the loss of mass expressed in percent m/m. Two
gram of the powder was weighed accurately and transferred into a dry Petri dish. The
Petri dish is placed in a desiccator for 2 days over calcium chloride crystals. Then the
powder was taken and weighed accurately to find out the weight loss during drying
[26].
10. Moisture content: The moisture content is determined by heating a shampoo at
105oC in a hot air oven to a constant weight. 1 gm of Shampoo weigh in crucible and
heat on steam bath for 30 min. Continuous heating at 105 oC in oven for 24 hrs, cool
in desiccator [26].
11. Ash content: Weight about 5 ml of shampoo in flat bottom Petri dish and heat on
steam bath under jet of air for 1 hour. Remove and add 1 g of ash less cellulose
powder, keep the material in dish and heat in a 1 K heating lamp till 600 oC in muffle
furnace.
Standard Value= 0.03-0.07% [26].
12. Viscosity: The viscosity of the tested shampoos was determined using the Brookfield
Viscometer (R/S plus rheometer model, LV, USA) set at different spindle speeds of 1–
 5, 10, and 20 rpm. The shampoos’ viscosities were measured using spindle C50-1. The
temperature and the sample containers’ sizes were kept constant [9].
13. Microbiological contamination: Shampoo is a cosmetic product that directly comes
in contact with the human scalp; hence, it is expected to be free of any
microbiological contamination. Microbes as gram-negative bacteria and total viable
count (TVC) of microbes are absent in all the shampoos tested. Microbiological tests
are used to evaluate the microbial contamination of hair shampoos. These tests
include total viable count, total yeast and mold count, and identification of specific
microorganisms. In addition, tests for endotoxins and mycotoxins may also be
performed [20].
14. Chemical tests: Tests are performed to determine the chemical composition of hair
shampoos. The total active ingredients of hair shampoos can be measured using
techniques such as high-performance liquid chromatography (HPLC) or gas
chromatography (GC). Sodium lauryl sulfate (SLS) is a common ingredient in
shampoos, and its concentration can be measured using HPLC or GC techniques.
Other chemical tests may include the measurement of preservatives, fragrances, and
other additives [20].
15. Stability studies: The thermal stability of the shampoos was studied by placing them
in glass tubes in a humidity chamber at 45 °C with 75% relative humidity as well as in
a refrigerator at 4 °C, and comparing them to the same shampoos kept at a room
temperature of 25 °C. The thermal stabilities were observed after storage periods of
zero, four, and eight weeks. Their appearances and physical stabilities were inspected
for a period of two months [9].
Recent advances in quality control (QC) testing for shampoos have focused on
developing more sensitive and accurate methods for evaluating the physical, chemical, and
microbiological characteristics of these products.

One recent study evaluated the use of near-infrared (NIR) spectroscopy for the
quantitative analysis of hair shampoos. Results showed that NIR spectroscopy can provide
accurate and reliable measurements of key characteristics, such as pH, viscosity, and total
surfactant concentration, in a rapid and non-destructive manner [21]. Another study
investigated the use of microfluidic paper-based analytical devices (µPADs) for the
detection of SLS, a common surfactant in shampoos. Results showed that µPADs can
provide a simple, rapid, and cost-effective method for the quantitative detection of SLS in
hair shampoos. In addition, studies have also focused on the development of more sensitive
methods for the detection of microbial contamination in hair shampoos [22].

Studies evaluated a novel method for the detection of microbial contamination using a
combination of PCR and DNA sequencing techniques. Results showed that this method
can provide a more sensitive and accurate detection of microbial contamination compared to
traditional culture-based methods [24]. Studies evaluated the use of a microfluidic chip-
based system for the rapid and sensitive detection of microbial contamination in hair
shampoos. Results showed that this system can detect low levels of bacterial contamination
in just 2 hours, compared to traditional methods that can take several days [23].

Studies investigated the use of a portable Raman spectroscopy system for the rapid and
non-destructive analysis of hair shampoos. Results showed that this system can provide
accurate measurements of key characteristics, such as pH, viscosity, and surfactant
concentration, in just a few minutes [25]. Studies investigated a portable, electrochemical
biosensor for the detection of microbial contamination in hair shampoos. Results showed
that this biosensor can provide a sensitive and specific detection of microbial contamination,
with a detection limit as low as 10 CFU/mL [18]. Overall, these recent developments in
quality control testing for hair shampoos are aimed at improving the accuracy, speed, and
sustainability of these methods. These advances are important to ensure the safety and
efficacy of hair shampoos for consumer use.

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