RESEARCH AND DEVELOPMENT DEPARTMENT

Davao Bioskin Tech Laboratories Inc.

PRODUCT STABILITY TESTING

PURPOSE

The purpose of stability testing of cosmetic product 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
is economically and efficiently addresses the testing required.

Because of the wide variety of cosmetics products “standard” stability test cannot be prescribed. Research
and Development Department require the flexibility to modify testing protocols an to build a scientific
basic for assessing stability of our own products. Thus, specific test may be developed in order to address
new or unusual technologies, or to be adapted to products having extended shelf lives. Stability test can
be conducted in real time or under accelerated conditions and should address the stability of the product
under appropriate conditions of storage, transport and use.

Basically, there are three (3) forms of stability tests: Physical and Chemical Tests which evaluate the 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, molds, and
yeast; and Packaging Stability Tests which evaluate the impact of packaging on the contained products.

TESTING PROCEDURE

Research and Development must set their own procedures on how to conduct stability test for cosmetic
products. Below are the steps that must be followed in product stability testing.

Step 1: Make Batches: Calculate how much to make based on the number of samples that will be using
for the test. (Container size, Conditions to be tested, available raw materials)

Step 2: Fill the Samples: Ideally the correct packaging must be fill in. When appropriate, fill glass jars (Glass
is the most inert material and does not react with cosmetic product in any way.) with the product along
with its final packaging. In this way it will be determined if the cause of product failure is the formula or
the packaging itself.

Step 3: Take Initial Readings: Once the samples are filled test it for all the characteristics that will be going
to evaluate later. Physical and chemical tests must be recorded. The exact tests depend on the product to
be tested.

Step 4: Put samples in different conditions: Stability testing required different temperature and light
conditions. Some standard temperatures include 50°C, 45°C, 37°C, 25°C (Required Temperature), and 4°C.
Freeze and Thaw stability test involves cycling the product through 24 hours of freezing then 24 hours of
thawing. Different lighting conditions involve a fluorescent light box and a natural light box (to stimulate
sunlight).

Step 5: Evaluate the product: Sample should be evaluated at the following intervals. 2 weeks, 4 weeks, 8
weeks, 12 weeks, and 52 weeks. The highest temperature samples and the light exposed samples only
need to be evaluated for the first three test intervals. The evaluation test should be the same as your
initial reading.

Step 6: Determine Stability: The decision whether the formula is stable or not will run 4-8 weeks or it will
vary depending as to what will be the outcome of the test. All products will exhibit some change so it will
still up to the Head of the Research and Development to decide whether the product will be passed or
not.

MICO JOHN ANDRES 1

 RESEARCH AND DEVELOPMENT DEPARTMENT
Davao Bioskin Tech Laboratories Inc.

STABILITY TEST PARAMETERS

The stability studies on cosmetic products are designed to ensure that the product or modified versions
meet the intended physical, chemical and microbiological quality standards as well as functionality and
aesthetics when stored under prescribed conditions. Such tests fall under three classes:

1. Physical and Chemical Tests: Appearance, color, odor/fragrance, viscosity, texture, flow and
emulsion stability, density, light stability and pH.
 Light Exposure Test often leads to discoloration of the product or the packaging/label.
 Centrifuge test is used to test stability of emulsion. Separation of emulsion layer or of oil
droplets is referred to as creaming. The emulsion is heated to 50°C and centrifuge for 30
min at 3000 rpm.
 Freeze – thaw cycling Test is done at 0°C or -10°C. Product is kept at -10°C for 24 hours
and at 25°C for next 24 hours (referred to as cycle). A product passing these cycles tests
is considered stable. If the temperature is cycled between -10°C and 45°C for three 24-
hour cycles is considered to be a high-quality product.
 Mechanical shock test is done to determine if the shipping movements can damage the
product or its packaging at different stages of such test’s measurements can be made for
color, fragrance, viscosity, pH value, particle size, etc.
2. Microbiological: Microbiological contamination can result during manufacture, transportation or
during usage by consumer. Contamination includes with growth of bacteria, mold and yeast.
 Screening test using rapid semi qualitative or quantitative test involving enrichment
culturing and colony counting are often employed if necessary.
3. Packaging Compatibility: Integrity of the package and the product under the expected condition
of storage and transportation. Test on packaging include leakage test, weight loss tests, and
testing in inert containers.
 Weight Loss Tests is to determine the 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 45°C for a period of 1 month. The
weight loss should not exceed 1% 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).

MICO JOHN ANDRES 2

 RESEARCH AND DEVELOPMENT DEPARTMENT
Davao Bioskin Tech Laboratories Inc.

PRODUCT STABILITY TESTING AND SAMPLING REPORT

PRODUCT NAME :
DATE :
SAMPLE :
R&D SPECIALIST :

GENERAL INSTRUCIONS : Product stability testing and sampling is solely responsibility of the Research
and Development Team. The specialist must record all results in accordance with the tests being use
during the experiment. This Report will be validated by the Research and Development Head and will be
approved by the upper management.

PHYSICAL AND CHEMICAL TESTS (INITIAL READING)

These describes approaches to predicting how well cosmetics will resist common stresses such as
temperature extremes and light. It will determine whether to perform such specialize testing based on
the vulnerabilities of the particular cosmetic product and its anticipated shipping, storage display and use
conditions.
CONTROL SAMPLE
Appearance :
Color :
Odor/Fragrance :
Viscosity :
pH :

CYCLE TEST/FREEZE – THAW TEST

The product should pass three cycles of temperature testing from -10°C to 25°C. Place the product at
-10°C for 24 hours and place it at room temperature 25°C for 24 hours. This complete once cycle. If the
product passes three cycles then it will have a good degree of confidence in the stability of the
product.

OBSERVATION
Color:
Cycle 1 (-10°C to 25°C) Odor:
Viscosity:
24 Hours pH:
Color:
Cycle 2 (-10°C to 25°C) Odor:
Viscosity:
24 Hours pH:
Color:
Cycle 3 (-10°C to 25°C) Odor:
Viscosity:
24 Hours pH:

MICO JOHN ANDRES 3

 RESEARCH AND DEVELOPMENT DEPARTMENT
Davao Bioskin Tech Laboratories Inc.

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 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 50°C 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 kinds such as liquid/cream make-up.

OBSERVATION
Color:
Odor:
Viscosity:
pH:

IS there a trace or sign of creaming after the test? YES NO

LIGHT EXPOSURE TEST

Both Formulas and packaging can be sensitive to the UV radiation. All products should be placed, in a
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 to serve as a control. All too often
you can 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 raw materials (e.g. 0.1% of benzophenone)
OBSERVATION
Color:
Odor:
Viscosity:
pH:

IS there a trace or sign of discoloration after the test? YES NO

Please Note the factors that causes the discoloration of the product:

MICO JOHN ANDRES 4

 RESEARCH AND DEVELOPMENT DEPARTMENT
Davao Bioskin Tech Laboratories Inc.

MECHANICAL SHOCK TEST

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 the separation of granular products is likely to occur.

OBSERVATION
Color:
Odor:
Viscosity:
pH:

IS there a trace or sign of separation after the test? YES NO

Please note the different factors observed during the test.

MICO JOHN ANDRES 5

 RESEARCH AND DEVELOPMENT DEPARTMENT
Davao Bioskin Tech Laboratories Inc.

PACKAGING STABILITY TEST

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. fragrance) may evaporate through the container.

GLASS TEST

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 we can determine if the cause
of product failure is the formula or the package.

OBSERVATION

WEIGHT LOSS TEST

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
45°C for a period of 1 month. The weight loss should not exceed 1% for the package to be considered
acceptable.
OBSERVATION

FORMULATION FOR WEIGHT LOSS

WL = TN1/TN2 x 100%

Where:
WL = Weight Loss
TN1 = total weight of the product
TN2 = total weight of the product after test

MICO JOHN ANDRES 6

 RESEARCH AND DEVELOPMENT DEPARTMENT
Davao Bioskin Tech Laboratories Inc.

LEAKING TEST

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).

OBSERVATION
Position Positive (+) Negative (-)
Upright

Inverted

Side

MICO JOHN ANDRES 7

 RESEARCH AND DEVELOPMENT DEPARTMENT
Davao Bioskin Tech Laboratories Inc.

QUALITY ASSESSMENT FORM

GENERAL INFORMATION
PRODUCT NAME:
DATE:
SAMPLE BATCH:
R&D SPECIALIST:
PART I. SAMPLE PRODUCT SAFETY INFORMATION
Please indicate all the information needed
1.1 QUALITATIVE AND QUANTITATIVE COMPOSITION OF THE SAMPLE PRODUCTS
The complete product composition must be specified stating the trade name and any other identity
(qualitative) of each raw material including an indication of the amount of each raw material stating
weight percentage (quantitative).
CHEMICAL IDENTITY
RAW MATERIAL
FUNCTION PERCENTAGE NAME OF SUPPLIER
(INCI NAME)

1.2 PHYSICAL/CHEMICAL CHARACTERISTICS AND STABILITY OF THE SAMPLE PRODUCTS

The physical and chemical characteristics of the substances or mixtures as well as the cosmetic
product. The stability of cosmetic product under reasonably foreseeable storage conditions.
TESTS PARAMETERS RESULT
1. Cycle Test/Freeze-Thaw Test
2. Centrifuge Test
3. Light Exposure Test
4. Mechanical Shock Test
5. Glass Test
6. Weight Lost Test
7. Leak Test
8. Microbiological Test
1.3 EXPOSURE TO THE SAMPLE PRODUCTS
Data on the exposure to cosmetic product taking consideration the findings under sample feedback
form.
EXPOSURES RESULT
1. Site of Application (Face,
Body, etc.)
2. The amount of Product
applied.
3. The duration and frequency
of application.
PART II. COSMETIC PRODUCT SAFETY ASSESSMENT
1.1 FDA CONCERNS
List of Raw Materials that are
banned or with regulation of
Use.
Product is already registered
1.2 ASSESSMENT CONCLUSION

PREPARED BY REVIEWED AND VALIDATED BY

Research and Development Specialist Research and Development Head
APPROVED BY
MANAGEMENT

MICO JOHN ANDRES 8

 RESEARCH AND DEVELOPMENT DEPARTMENT
Davao Bioskin Tech Laboratories Inc.

PREPARED BY REVIEWED AND VALIDATED BY

Research and Development Specialist Research and Development Head
APPROVED BY
MANAGEMENT

MICO JOHN ANDRES 9