evaluation of cosmetics seminar.ppt

EVALUATION OF
COSMETIC MATERIAL
Presented by
Shaik Mohammed
M.Pharm 1st Year
Herbal and Cosmetic Analysis
Department of Pharmaceutical Analysis

INTRODUCTION TO
COSMETICS
• Cosmetics are defined as “articles intended to be rubbed, poured,
sprinkled, or sprayed on, introduced into, or otherwise applied
to the human body for cleansing, beautifying, promoting
attractiveness or altering the appearance”
• They include products such as skin moisturizers, perfumes,
lipsticks, fingernail polishes, eye and facial make up preparations,
shampoos, hair colors, toothpastes, deodorants as well as any
material intended for use as a part of cosmetic product.
• “Evaluation of cosmetic raw materials and finished products” are
carried out to meet the criteria of safety, properly labeled products,
using no prohibited ingredients and adhering to limits on restricted
ingredients

STUDY OF QUALITY OF RAW
MATERIALS

Raw materials used in cosmetics
1. Water
2. Preservatives
3. Humectants
4. Surfactants
5. Oils, Fats and Waxes
6. Perfumes
7. Colorants.

1. WATER
• Most widely used raw
material in the manufacture
of cosmetics.
• Water is used as a solvent
for many ingredients of
cosmetics.
• Water contains inorganic
ions like Ca, Mg, Na, K,
HCO3, SO4, Cl, silicates,
etc.
• Water is cheap, abundant
and innocuous.
Water will be contaminated by
• Presence of inorganic ions -
Mg and Zn may interfere with
static charges of surfactant and
it seperates the emulsion
• Presence of Micro
organisms- if microorganisms
are present in the formulation
of cosmetics then leads to foul
odour, visible colonies of
bacteria, mould, or fungi. This
may harm the cosmetics

Purification of water
 Distillation / Double distillation
 Ion exchange system
 resins are used- to remove cations and anions to form de-ionised water.
 columns are made up of resins can be regenerated
 Reverse Osmosis - 75% purified water collected and 25% as
concentrated water. Membranes are made up of cellulose
nitrate and poly amide.
Boiling Steam Condensation

Microbiological purification
 Chemical treatment - chlorine (1-4ppm) to de-
ionise water,HCHO also used.
 Heat treatment - boiling- held it for 20 minutes.
for spores - boiling after 2hrs.
UV radiation- below 300nm - lethal effect on
microbes.
 Filtration - membrane filters.

2. PRESERVATIVES
• Preservatives are used to
prevent the spoilage of
cosmetics.
• Spoilage occurs because of
two reasons
– Oxidation of oils and fats
– Microbial growth
• Absence of preservative causes
deterioration.
• Preservatives
– Anti-microbial.
– Anti- oxidants.

Anti-microbial:
the agents that are used to prevent or inhibit the
formation of microorganism(bacteria,fungi,yeast)
over the cosmetic products.
contaminated cosmetics usually contains -
staphylococci, diptheroids, fungi , yeast
Sources of microbial agents
1. raw materials
2. environment
3. equipment
4. packaging material
5. personnel

Ideal properties of preservatives
• Compatible with formulation
• Extent of solubility
• Stability
• Should give sustained anti-microbial effect
• Colorless & Odourless
• Non- toxic, Non-irritant, Non-allergic

Classes of preservatives
i. Organic acids
• Benzoic acid
• Formic acid
• Vanillic acid
• Propionic acid
• Sorbic acid
ii. Alcohols
• Ethyl alcohol
• IPA
• Chlorobutanol
iii. Aldehydes
• Formaldehyde
• Cinnamic aldehyde
iv. Phenolic compound
• cresol
• phenol
• p-cloro-m-cresol
• p-chloro-m-xylenol
v. Esters
• Methyl p- hydroxy benzoate
• Ethyl p- hydroxy benzoate
• Propyl p- hydroxy benzoate
• Butyl p- hydroxy benzoate
vi. Mercury compound
• Thiomersol
• Nitromersol
• Phenyl mercuric salts i.e.
nitrate, acetate.
vii. Surfactants
• BTC
• BAC
• Cetyltrimethyl
ammonium
bromide
viii. Inorganic comp
• Boric acid
• SO2
viii.Miscellaneous
• 5-bromo-5-
nitro-1,3-
dioxan
• Vanillin
• Ethyl vanillin

QC tests of some preservatives
Boric Acid
Boric acid is used in the formulation of a wide variety of product
types including creams and lotions and bath, hair and skin
products.
Assay of boric acid( H3BO3)
• Weigh 2gm of boric acid + 50ml of water + 100ml of glycerin
• Neutralized with phenolphthalein
• Titrate against 1M NaOH
• End point is appearance of faint pink color
Each 1ml of 1M NaOH = 0.06183gm of boric acid

Assay of Methyl paraben
Category- Anti -Microbial preservative
• 80mg Methyl paraben + transfer to a glass stoppered flask+ 25ml 2M
NaOH + boil for 30 min
• Cool + 25ml 0.03M KBr +5ml 12.5% w/v soln KBr + 40ml glacial acetic
acid
• Cool in ice + 10ml HCl
• Allow to stand for 10 mins + 15ml KI soln and titrate liberated I2 with
0.1M Na2S2O3 using starch soln indicator
• Perform blank
• Difference between titrations represents the amount of KBrO3 required
• Volume of KBrO3 is equivalent to half of volume of Na2S2O3 required for
titration
KBrO3 = 0.005 gm Methyl paraben

Anti-oxidants : to prevent the oxidative deterioration in cosmetics.
Example: Ascorbic acid, Citric acid, Sodium metabisulphite etc.,
 Rancidity(smelling or tasting like rank stale fat)
-occurs due to oxidation of fats and oils.
 Classification of Anti-oxidants
1. Phenolic type (gallic acid, methyl gallate, butyl p-hydroxy
benzoate)
2. Quinone type (tocopherols, hydroxy chromans)
3. Amine type(lecithin, ethanolamine)
4. Organic acids, alcohols and esters(ascorbic acid,citric acid,
oxalic acid)
5. Inorganic acids and their salts(sodium sulphate, sodium meta
bisulphate)

QC tests for some anti oxidants
Assay of citric acid:
•weigh 1.5gm citric acid +
25ml water - from this, pipette
25ml and make up to 100ml
with water .
•Titrate against 0.1M NaOH
using phenolphthaein
indicator.
•End point is appearance of
faint pink color
Assay of Ascorbic acid:
 Weigh 0.1gm + dissolve in
25ml of freshly boiled water
+ 1ml of H2SO4
 Titrate against 0.05M
Iodine using starch as
Indicator
 End point is blue color that
persists after 20 seconds of
swirling the solution
Each ml of 0.05M Iodine =
20.49gm of Ascorbic acid

3.HUMECTANTS
 Hydrating substance used in
cosmetics products to retard
moisture loss and increase the
moisture content in skin that is in
contact with the products.
 Target area in the body for
treatment with humectants are dry
skin.
 Hydration play an important role
in maintaining the metabolism,
enzyme activity, mechanical
properties, appearance, and finally
barrier function of skin.

Types of humectants
1. Inorganic humectants(limited use, corrosive Nature)
– Example : Calcium Chloride
2. Metal organic humectants (limited use)
– Ex: Sodium Lactate
3. Organic humectants
– Polyhydric alcohols
• ethylene glycol
• propylene glycol
• glycerol
• PEG

4.SURFACTANTS
 A surfactant or surface active agent is a
substance that, when dissolved in
water, gives a product the ability to
remove dirt from surfaces such as the
human skin, textiles and other solids.
 Surfactants are wetting agents that
lower the surface tension of liquid,
allowing easier spreading, and lower
the interfacial tension between two
liquids.
 Surfactants functions as:
 Emulsifiers
 detergents, foaming, cleaning
agents
 wetting agents
 solubilizers
HOW SURFACTANTS WORK

Surfactants
 Molecules with both a polar and a
non-polar end polar portion is
hydrophilic (water- loving).
 non-polar, hydrocarbon end is
hydrophobic (water hating or
fearing) or lipophilic (oil-
living).....CH3CH2CH2CH2CH2C
H2-etc.

Classification of Surfactants
 Anionic - it carries negative
ion in solution
– Ex - Sodium oleate -
C17H33COO+Na-
 Cationic - It carries positive
ion in solution
– Ex - Alkyl trimethyl
ammonium salts
 Non- ionic - hydrophilic
uncharged polar groups
– Ex - Alkyl polyglycol
ethers
 Amphoteric - it carries both
ions in solutions
– Ex: Acyl peptides betains

5. OILS,
FATS and WAXES
OILS
Vegetable origin
Mineral origin
Vegetable oils
 Almond oil : Emollient properties used in creams and
lotions
 Arachis oil : Used in hair oils as brilliantines
 Castor oil : used in Lipsticks, hair oils, creams.
 Olive oil : Emollient and Soothing, used in Bath oils,
Creams.
 Coconut oil

Mineral oils
 Light liquid paraffin: used in bath oils, lotions, and creams.
 Heavy liquid paraffin : Emollient in nature, used in creams, lotions,
hair oils, bath oils
FATS
Fatty acids
Oleic acid is used for enhancing pearly shine in lotion and creams
Fatty alcohols
Lauryl alcohol and myristyl alcohol used in creams and lotions.
Fatty acid esters
Glyceryl monostearate, ethylene glycol monostearate(0.5%- 5% in
lotions & 1- 10% in creams)
Lanolin and its derivatives
used as a emulsifier in w/o type emulsion

SOFT PARAFFINS
 Purified mixture of hydrocarbons obtained from
petroleum
Act as a emollient and prevents water loss from the
skin and promoting its hydration
WAXES
Animal wax - bees wax, lanolin, spermaceti
Plant wax - Carnuaba, Candelia
Mineral wax - Ozokerite, Paraffin, Ceresin
Synthetic wax - Polyethylene, Carbowax

Uses of OILS,FATS and WAXES
• Oils and fats used in cosmetics are obtained from animals or
plants and they are processed to remove the smell and odour.
• Used in cosmetics as film forming agents, moisturizers, to
improve the feel and some others are used as nourishing oils
• Volatile oils used in cosmetics are mostly used as fragrant
additive
• Waxes used in cosmetics are to give a hardening and
thickening effect

6. PERFUMES
Perfumes are a mixture of fragrant essential oil, Aroma
Compounds, Fixatives, and Solvents used to give the human
body, objects and living spaces a pleasant smell.

Natural ingredients:
 Flowers : Rose, Jasmine,
Osmanthus, Mimose,
Tuberose
 Fruits: Orange, lemon, grape
fruits
 Seeds : Coriander, Caraway,
Cocoa, Cardamom, Anise
 Wood : Sandalwood,
Rosewood
 Roots : Roots of ginger
family
 Resins : Peru balsams, gum
benzoin, pine and Fir resins
 Leaves : Lavender leaf, Rose
mary, Citrus leaves

Animal sources
Castor comes from beavers,
Musk from Male deer,
Ambergris from whale’s sperm.
FIXATIVES
• Animal sources often used as fixatives that enables
perfume evaporate slowly and emits odour longer.
• Various animal products as fixatives: Ambergis,
musk, castoreum, civet.
eg. Ambergis compound from sage

Perfume odorant types :
Concretes
Purest, soft plant parts are placed in a solvent
Absolutes
concretes concentrated in alcohol
Resinoids
Extracted like concretes, from plant secretions
Tinctures
Direct extraction with ethanol
Distilled essential oils
Most common modern methods

Types of fragrances:-
• Perfume (22% essential oils)
• Eau de Parfum (15-22%)
• Eau de Toilette(8-15%)
• Eau de Cologne(4%)
PERFUMES SOURCE USES
LAVENDER LANGUSTIFOLIA / MINT
FAMILY
MEN’s FRAGRANCES
ROSE ROSA CENTIFOLIA PERFUMES and FOODS
GERANIUM Pelargonium graveolens Insect repellent
JASMINE Jasminum grandiflorum Used to be enfleurage
ORANGE Citrus species Perfumes

7.COLORS
• A generic term for any color imparting substance
CLASSIFICATION OF COLORS
1. Colorants : Substances soluble in the medium which is to be
used.
2. Pigments and color lakes: insoluble in the medium but
coloring achieved by uniform distribution.
3. Color lakes: Produced by precipitation of water soluble
colorant with aluminum hydroxide.
4. Water dispersible pigments : dispersed with the help of a
dispersing agents
5. Color additive: dye, pigment derived from a vegetable
derivative

6. Chrome: vividness of a color
7. Opacity : Degree of impenetrability by light
8. Bleed : Leaching of an impurity or minor
constituent from a colored article.
CLASSES OF COLORS EXAMPLES
NATURAL COLORS Cochineal,saffron, chlorophyll, henna, beet extract,
caramel colouring and carrot oil
INORGANIC COLORS iron oxides, chromium oxides, carbon black,
titanium dioxide, zinc oxide
ORGANIC COLORS amaranth, indigocarmine, orange G

Types of coloring agenta Cosmetic product used
Water Soluble colorants bath products, creams, soaps, toothpastes
and gels
Oil soluble Colorants and pigments face make up, lipsticks, soaps
Color lakes Eye make up, Lipsticks
Water dispersible pigments soaps

• According to D&C act, coal tar cannot be used in cosmetics.
• This rule further prescribes that Schedule Q colours should not
contain more than
– 2ppm of Arsenic trioxide
– 20ppm of Lead
– 100ppm of Heavy metals other than lead.
US approved organic colors:
Us approved colors are designated as
• FD&C : certified for use in food, drugs and cosmetics
• D&C : certified for use in drugs & cosmetics including in those in
contact with mucous membranes and those that are ingested
• Ext. D&C : certified for use in drugs & cosmetics that do not come
in contact with mucous membranes or those that are ingested.

Selecting Colorants based on
Regulations
Products that Products which color should be
used
do not come into mucuous
membrae or eye area
shampoo,
conditioner,
hand cream
FD&C, D&C or Ext. D&C
colors
are used around the mouth Face cream ,
lipsticks
FD&C or
specifically approved D&C
colors
are used around the eye Mascara, Eye shadow only inorganic or natural
color or specifically
approved organic
colors(eg. FD&C Yellow 5)

 Selecting Colorants based on Formulations:
• Color selection depends also on the properties of a formulation
• Liquid products :(shampoo, lotion)
– use water soluble D&C or FD&C colors
• Solid products : (powders)
– Use inorganic or insoluble organic colors(lakes)
 Some colours permitted to use in cosmetics under Schedule
Q are
Tartrazine
Sunset yellow
Amaranth
Brilliant blue
Eosin TS

QC test for some colors
S. NO NATURAL
COLORANT
PROCEDURE INFERENCE
1 Cochineal test material +amyl alcohol+ dil
ammonia --------> shake
PRINCIPLE:
Carminic cid in cochineal
converted to ammonium
carminate
purple color
indicates the
presence of
cochnieal
2. Caramel Fiehe’s Reaction :
sample soln+ 50ml ether--------
evaporate in residue----- to the
residue + 3drops resorcinol in
HCl
rose color indicates
presence of
caramela
3 Chlorophyll sample - extracted with ether +
10% ethanol
extract turns brown
and quickly returns
to green.
this shows presence
of chlorophyll

S.NO INORGANIC
COLORANTS
PROCEDURE
1 Titanium dioxide • Sample in kjedhal flask+ 5 anhydrous. Na2SO4+10ml
water+ 10ml H2SO4----- boil till clear liquid---- cool +40ml
cooled 25% H2SO4-- cool again -- dilute with water to
100ml (soln B)
• 300g Zn + 300ml 2% w/v Mercuric nitrate + 2ml HNO3 --
shake for 10minutes---- wash----- pack Zn amalgam into
glass tube fitted with tap and filter plates at a rate 3ml/min
--- +100ml 1M H2SO4 +100ml water-- pass slowly through
column(3ml/min) +200ml 0.5M H2SO4 + 100ml water ---
collect combined eluates+ 50ml 15% w/v FAS in H2SO4 -
titrate with 0.1M cerric ammonium nitrate(using ferroin
as indicator)--------------> green (n1 ml)
• then pass slowly 100ml 0.5M H2SO4 & 20 ml soln B
through column-- wash it 100ml 0.5M H2SO4 and 100ml
water --collect-- combined eluates + 50ml 15% w/v FAS ---
titrate with 0.M CAN using ferroin as indicator ------>
green (n2 ml)
% TiO2 = 3.99 (n2-n1)/ W

S.NO INORGANIC
COLORANT
PROCEDURE
2. ZnO
• It is a white
pigment
• it is high in
brightness and
low in tinting
strength
• it finds extensive
use in face
powder
0.15g sample + 10ml 2M acetic acid --------> dilute
with 50ml water + 50mg xylenol orange titrate &
sufficient hexamine (to produce violet pink) + 2
hexamine ---> titrate with 0.1M disodium EDTA to
yellow color endpoint
1M disodium EDTA = 0.008138g of ZnO

General Methods of Analysis of
Raw materials used in
Cosmetic Manufacture as per
BIS

 Bureau of Indian Standards (BIS) has done commendable
works in fixing specifications for many raw materials used in
cosmetics.
 The tests normally involve physical parameters (color, odour,
density, refractive index, viscosity, etc.) and chemical
parameters (assay of active ingredients, impurities present,
etc.) and these chemical parameters determination varies
depending upon the specific type of raw material used.
 Drugs and cosmetics act specifies the limits of impurities in
cosmetic raw materials like lead, arsenic and heavy metals

Tests for Identification and Quality:
Physical Analysis:
•Organoleptic properties:
a) Appearance: Appearance must be checked with that of the standard and
can be done by visual inspection.
b) Color: color of the raw material used must meet the specifications of the
standards. For example the color of fatty acids is designated as a photo metric
index expressed as 100 x the absorbance at each of two wavelengths, 440 and
550 nm.
c) Odour: The demand for product stability, accompanied by a requirement
for bland-smelling products, is increasing for raw materials also. This is
probably a result of their use in cosmetics and they must meet the standard
specifications.

Physical Characteristics:
a) Specific gravity:
The specific gravity can be determined by dividing the mass of the substance to be
determined to the mass of the water.
b) Refractive index:
• It is not only useful for identification purposes and for establishing purity, but also for
observing the progress of reactions of fatty acids, such as catalytic hydrogenation and
isomerization.
•The refractive indices of fats and fatty acids increase with number of double bonds and
with increase in conjugation.
•Refractive index of a substance is determined by the ratio of the velocity of light in
vacuum to its velocity in the substance to be determined which varies according to the
sample.
c) Melting point, Freezing point, Cloud point:
The determinations of these specific values are used to identify the quality of the
sample as they are specific to particular type of the compounds.

d) Viscosity: This can be determined by the use of different types of
viscometers by which resistance offered by a particular sample to flow
is determined.
e) In addition to the above, different physical characteristics are also
determined based on the type of raw material to be evaluated.
Chemical Analysis:
In the case where fats and oils are used as raw materials different tests such as
saponification value, acid value, iodine value, and unsaponifiable matter,etc..
can be performed to determine their quality.
a) Saponification value and Hydroxyl value: This is the number of free
hydroxyl groups occurring in the oil or fat, i.e. in the mono- and diglycerides,
hydroxy acids, etc.
b) Iodine value: If the fat or oil contains unsaturated fatty acids, the iodine
value can be used as an identification method. If not, it can be used as a test for
unsaturated impurities.

c) Unsaponifiable matter: Different natural oils and fats contain known
specific unsaponifiables, e.g. sterols or vitamins. Isolation of these from the
fatty material can be used to identify the oil or fat. When testing named
materials, unexpected unsaponifiables indicate adulteration of the original
sample.
Assay: Assay of the raw material can be performed to determine its quality.
Tests for Impurities:
Trace Metals:
Recent developments in the technique of atomic absorption analysis have
been extraordinary.
This technique offers accurate, rapid analysis of trace metals without the
need for time consuming ashing steps.
The AOCS offers two atomic absorption spectrophotometric methods for
trace metals in the raw materials to used in the manufacture of cosmetics.

Modern Technological Methods for Identification and Quality
in Cosmetic Raw materials:
 Chromatographic Analysis:
 Different types of chromatographic techniques such as
Column chromatography, Thin layer chromatography, Ion
exchange chromatography, Gas chromatography, High
performance liquid chromatography can be utilized to
determine the quality of raw materials used in cosmetic
manufacture by their characteristic retention time and
retardation factor.
 The values of retention time and retardation factor of one
compound is specific when a particular type of
chromatographic method is employed which varies for another
compound and when different chromatographic method is
followed.

 Spectroscopic Analysis:
 By “IR spectroscopy” where based on the characteristic
functional groups present in the raw materials employed in the
manufacture of cosmetic the identity and presence of
impurities in the raw materials can be determined.
 In “Ultra violet spectroscopy” based on the characteristic
absorption of UV radiation by a particular raw material at a
particular wavelength is determined and is compared to the
standards to determine the quality and purity of the raw
material.
 In “Fluorescence Spectroscopy”, the fluorescence excited by
ultraviolet radiation has been suggested as an aid in the
identification of fats and oils in the case where they are used as
raw materials in the manufacture of cosmetics.

 For some of the more common acids the colors are as follows:
• Formic-palelilac;
• Acetic-colorless;
• Propionic_x0002_colorless;
• butyric-weak yellow;
• Caproic-red violet;
• Lauric-vivid violet palmitic-pale yellow-grey;
• Stearic-white with a violet tinge;
• Oleic-strong violet; etc.
 The colors of the fluorescence of natural oils depend upon that
of the acids which they contain and these have been used for
the detection of adulterants or contaminants.

 In “Nuclear Magnetic Resonance Spectroscopy”, the high
resolution nuclear magnetic resonance spectra of raw materials used
in cosmetics are produced.
 The peaks represent the protons with different types of chemical
bondings and the area below each peak reflects the number of
protons in each type of chemical bonding which can be used to
determine their quality and the presence of impurities.
 In addition to the above techniques, other spectroscopic techniques
can also be employed for the determination of quality of raw
materials used in the manufacture of cosmetic products.

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