Stability Testing of Cosmetics

The purpose of stability testing cosmetic products is to ensure that a new or modified
product meets the intended physical, chemical and microbiological quality standards as well
as functionality and aesthetics when stored under appropriate conditions. Because the
development cycle of cosmetic products is relatively short each manufacturer should design
their own stability testing program such that it is economically reasonable and efficiently
addresses the testing required.

Because of the wide variety of cosmetic products standard stability tests cannot be
prescribed. Manufacturers require the flexibility to modify testing protocols and to build a
sound scientific basis for assessing stability of their own products. Thus, specific tests may
be developed in order to address new or unusual technologies, or to be adapted to products
having extended shelf lives. Stability tests can be conducted in real time or under
accelerated conditions and should address the stability of a product under appropriate
conditions of storage, transport and use.
Basically, there are three forms of stability tests: physical and chemical integrity tests which
evaluate color, odor / fragrance, pH value, viscosity, texture, flow, and emulsion stability
(signs of separation); microbiological stability tests which evaluate the degree of
contamination with bacteria, mold, and yeast; and packaging stability tests which evaluate
the impact of packaging on the contained product.

Physical / Chemical Stability Tests

These describes approaches to predicting how well cosmetics will resist common stresses
such as temperature extremes and light. Typically, manufacturers determine whether to
perform such specialized testing based on the vulnerabilities of the particular cosmetic
product and its anticipated shipping, storage display and use conditions. Common test
procedures include:
Temperature Variations: High temperature testing is now commonly used as a
predictor of long-term stability. Most companies conduct their high temperature testing at
37oC (98F) and 45oC (113F). If a product is stored at 45oC for three months (and exhibits
acceptable stability) then it should be stable at room temperature for two years. Of course,
the product must be stored at 25oC (77F) for a period of one year. A good control
temperature is 4oC (39F) where most products will exhibit excellent stability. The product
should also be subjected to -10oC (14F) for three months.
Cycle Testing: The product should pass three cycles of temperature testing from
-10oC (14F) to 25oC (77F). Place the product at -10oC for 24 hours and place it at room
temperature (25oC) for 24 hours. This completes one cycle. If the product passes three
cycles then you can have a good degree of confidence in the stability of the product. An
even more rigorous test is a -10oC to 45oC five-cycle test. This puts emulsions under a
tremendous stress and, if it passes the test, indicates that you have a really stable product.
 Centrifuge Testing: The dispersed phase (of an oil-in-water emulsion) has a
tendency to separate and rise to the top of the emulsion forming a layer of oil droplets. This
phenomenon is called creaming. Creaming is one of the first signs of impending emulsion
instability and should be taken seriously. A good test method to predict creaming is
centrifugation. Heat the emulsion to 50oC (122F) and centrifuge it for thirty minutes at 3000
rpm. Then inspect the resultant product for signs of creaming. This test is an absolute
necessity for those products that contain powders of any kind such as liquid/cream make-
up.
Light Exposure Testing: Both formulas and packaging can be sensitive to the UV
radiation. All products should be placed, in glass and the actual package, in the window and
if its available a light box that has a broad-spectrum output. Place another glass jar
completely covered with aluminum foil in the window to serve as a control. All too often we
will see significant discoloration of the product and sometimes of the package also. This
discoloration may be due to the fragrance or some other sensitive ingredient. Usually all
that is needed is the addition of a UV absorber (e.g. 0.1% of benzophenone).
Mechanical Shock Testing: In order to determine whether or not shipping
movements may damage the cosmetic and its packaging mechanical shock testing is often
conducted. Vibration testing (e.g. on a pallet shaker) can help to determine whether de-
mixing (separation) of powders or granular products is likely to occur.
Monitoring: For all the above mentioned tests you should monitor the color, odor /
fragrance, viscosity, pH value, and, if available, particle size uniformity and/or particle
agglomeration under the microscope.

Microbiological Stability Tests

Microbial contaminants usually come from two different origins: during production and filling,
and during the use of the cosmetic by the consumer. From the moment the cosmetic unit is
opened by the consumer, a permanent microbial contamination of the cosmetic is
introduced caused by contact with the consumers hands and body.

Microbial preservation of cosmetics is important to ensure the microbial safety of cosmetics

for the consumer, maintain the quality of the product,and confirm hygienic and high-quality
handling. Although only a small number of cases of microbial infections of the consumer has
been reported, microbial contamination of cosmetic products may spoil them or seriously
reduce the intended quality.

Therefore, it is necessary to carry out routine microbiological analysis of each batch of the
finished product coming on the market. Pseudomonas aeruginosa, Staphylococcus Aureus
and Candida Albicans are considered the main potential pathogens in cosmetic products.
These specific potential pathogens must not be detectable in 0.1 g or 0.1 ml of a cosmetic
 product. The parameters examined, the criteria and methods used, and the results obtained
per batch should be documented.
Screening Tests: There are various easy testing kits available on the market (e.g.
dip-slides or plate counts) which provide quick and semi-quantitative results whether a
cosmetic product is significantly contaminated or not. Sampling and evaluation of the results
is simple and can be performed also by personnel without any microbiological training.
Quantitative Tests: Quantitative tests determine the actual count level of bacteria,
mold and yeast in a cosmetic product. These tests are very sophisticated and laborious and
can be performed only by professional microbiological testing laboratories. Typically,
methods for isolation of microorganisms from cosmetic products include direct colony
counts and enrichment culturing.

Packaging Stability Tests

Packaging can directly affect finished product stability because of interactions which can
occur between the product, the package, and the external environment. For example,
product constituents may be absorbed into the container or may chemically react with the
container. In addition, the container may not fully protect the product from the adverse
effects of atmospheric oxygen and/or water vapor, or volatile product constituents (e.g.
fragrances) may evaporate through the container.

Glass Tests: Glass is the most inert material and does not react with a cosmetic
product in any way. For this reason all testing should be done in glass and the actual
packaging. In this way you can determine if the cause of product failure is the formula or the
package.
Weight Loss Tests: To determine evaporation (water loss through the container wall
or closure gaps) weight loss evaluation is one of the most important tests that must be
conducted. This testing (performed in the actual package with the cap torqued to 100% of
target torque) is done at room temperature and at 45oC (113F) for a period of three months.
The weight loss should not exceed 1% per month for the package to be considered
acceptable.
Leaking Tests: It may be advisable to test the packaged product in various
orientations (upright, inverted, on its side, etc.) to determine whether the packaging may
leak (especially during transport)
 Preservation of Cosmetics
More than any other ingredients, preservatives are the most vilified ingredients and most
often called out as the worst ingredients you can use in a formula. However, preservation
is mandated by the FDA stating that products sold to the general public must be safe for
use when it is applied to the body and must be free of contamination.
Since personal care products are not made and used in sterile conditions microbes will
inevitably grow making the use of preservatives a must for almost all personal care
products. Even if a product may be free of contaminants at the time of production, the
product must still be preserved sufficiently to kill microbes that are introduced later by the
consumers themselves.

Natural, insufficiently preserved cream overgrown with mold.

Factors to Minimize Contamination

Key factors for the exclusion or minimization of microorganisms throughout a products life
cycle include the following measures:

Clean Equipment: Sanitize equipment thoroughly with isopropyl alcohol, chlorine or

another proven sanitizer. Heat steam (water above 100C) works also.
Clean Water: Use sterile, distilled or deionized water, but not tap water. Lower the
water activity (amount of free available water in a formula) by adding small amounts of
glycerin, sorbitol, propylene glycol, or butylene glycol to the water phase.
Formula Optimization: Create a hostile environment for microorganisms. For
example, adjust the pH of the water phase to the level where preservatives act best and
 enhance susceptibility of microbes towards preservatives by adding EDTA, citric acid,
sodium citrate, etridonic acid, sodium gluconate, or phytic acid.
Preservatives: Use a preservative or better a combination of preservatives that offer
broad-spectrum protection (kill bacteria and mold) and add the preservatives to the water-
phase or at the end of the the formula, but not the oil phase. Consider adding co-
preservatives including essential oils and fragrances that have antimicrobial properties
including clove, cumin, eucalyptus, lavender, lemon, thyme, sage, sandalwood, neem and
tea tree oils.
Packaging Optimization: Use packaging that effectively protects the formula and
minimizes contamination by the user. Consider filling products into containers that have a
dispensing system (e.g. airless dispenser bottles) and do not require the consumer to use
their fingers.

Common Preservatives

Below is a list of the most commonly used preservatives for personal care products. Most
preservatives are not used alone but in combination with others.

Parabens: Parabens including methylparaben, propylparaben, and butylparaben are

the most commonly used preservatives. They are very effective against most bacteria and
fungi. Their efficacy can be limited at pH values outside the range of 4-8. As research has
shown that some parabens can have an estrogen-like effect, this finding has fueled a fear
that the parabens in underarm deodorants and other cosmetics can migrate into breast
tissue and contribute to the development of tumors. However, no direct evidence of a causal
link between parabens and cancer, however, has been shown. A review of the data
available concluded it is biologically implausible that parabens could increase the risk of any
estrogen-mediated effects. The American Cancer Society also concluded that there was
insufficient scientific evidence to support a claim that use of cosmetics such as
antiperspirants increase an individual's risk of developing breast cancer, and that larger
studies are needed to find out what effect, if any, parabens might have on breast cancer
risk.
Urea Derivatives: Urea derivatives including imidazolidinyl urea and diazolidinyl
urea are effective against all types of microbes including bacteria, fungi, and mold. They
work in a wider ph range (3-9) than parabens and are therefore often combined with
parabens. They are also often used in surfactant systems.
Phenol Derivatives: Phenol derivatives like phenoxyethanol have been used in
cosmetics for many years and can be effective against a range of microbes. As they are not
 as effective as parabens and urea derivatives they are often combined with other
preservatives. Phenoxyethanol should not be used in formulas containing HE-cellulose or
non-ionic surfactants as its efficacy can be compromised.
Alcohols: Ethanol is a good preservative but it has to be used at high levels (at least
20%). Other alcohol derivatives like benzylalcohol, dichlorobenzyl alcohol are more effective
but are also typically combined with other preservatives. Like phenoxyethanol,
benzylalcohol should not be used in formulas containing non-ionic surfactants as its efficacy
can be compromised.
Quats: Quats (quaternary ammonium compounds) are ingredients typically used as
hair conditioning agents. However, many of them can kill microbes. This include ingredients
like benzalkonium chloride, methene ammonium chloride, benzethonium chloride and
quaternium-15. Quats work in a wide ph range (4-10) but their cationic nature makes them
less compatible with anionic surfactants.
Isothiazolones: Isothiazolones including methylchloro-isothiazolinone and methyl-
isothiazolinone are effective at already low levels. They work in a wide pH range and are
useful in a variety of formulation systems.
Other Preservatives: There are a variety of other preservatives including potassium
sorbate, sorbic acid, sodium benzoate, chlorocresol, chloroxylenol, chloracetamide,
triclosan, DMDM Hydantoin, and iodopropynyl butylcarbamate that all are effective against
some but not all types of microorganisms, or face other limitations.
Natural Preservatives: Based on the increasing demand for natural preservatives
the cosmetic industry is continuously searching for new natural compounds able to limited
the growth of microorganisms. So far, only a few effective natural preservatives have found
their way to the market including Orange-Lemongrass Blend, Honeysuckle Blend, and a
solution of peptides isolated from the bacteria Leuconostoc kimchii upon fermentation of
radishes.

Expected Shelf Life

Unfortunately, it is not possible to accurately predict the shelf-life of a product that has been
preserved with a certain preservative since the shelf-life depends on various factors
including:

The type of formula and the ingredients used (whether and how much it contains free
water)
The circumstances under which the product has been produced (how well the tools
have been disinfected)
 The purity of ingredients (whether microbes have been introduced by contaminated
ingredients)
The storage conditions (temperature, sun exposure, humidity)
Whether or not the product will be dispensed "finger-free" (e.g. by a pump, disk
dispenser, or airless pump)
If a product has been produced under optimum conditions, contains a broad-spectrum
preservation system, is stored adequately, and dispensed "finger-free" a shelf-life of 2-3
years can be expected. However, the determination of a shelf-life should never be based on
assumptions but solely on bacterial stability testing.