Stability Testing:

Theory into
Practice
David Clarke BSc (Hons), MSc
Physics

Stability Testing: Theory

into Practice
Regulations overview
Objectives of Stability Testing
Testing Protocols
Interpretation of results

Regulations Overview
Cosmetic Product must be safe for human health
Proven by Cosmetic Product Safety Report (CPSR)
Report included in PIF

Part A Cosmetic Product Safety Information

Quantitative & qualitative composition

Physical/chemical characteristics & product stability
Microbiological quality
Impurities, traces, packaging information & packaging
stability
Normal/foreseeable use
Product/substance exposure
Toxicological profile
Undesirable/seriously undesirable effects
Other information

Part B Cosmetic Product Safety Assessment

Conclusions from Part A

Regulations Overview
Labelling
Date of Minimum Durability

If Date of Minimum Durability exceeds 30

months
PAO

Regulations Overview
Vague requirements
Testing conducted should be specific to the
product and the type of data required from it.

Objectives of Stability
Testing
Definition Determine whether a particular
formulation, in its immediate packaging
can retain its intended physical & chemical
stability and microbiological quality,
including its intended function and
aesthetics under the conditions of the
market in which it is to be sold.
Understand how the product shall fair over
time
Primary concern safety
Secondary concern Brand / Manufacturer
reputation
At what point are changes unacceptable?

Objectives of Stability
Testing
Product Stability Product stored and tested
in inert, impermeable glass jars
Container Compatibility Product and the
final, immediate packaging tested together
Recommend conducting both stability and
compatibility
Determines product or packaging instability

Types of Stability Tests

Real Time Stability Testing
Stored in actual market conditions for the
duration of minimum durability
Ensure test frequency is sufficient
Benefits real time degradation
Disadvantages - time

Types of Stability Tests

Accelerated Stability Testing
Stored under various conditions to accelerate
changes occurring under normal conditions
predicts stability
Benefits data acquired relatively quickly
Disadvantages
Instabilities in real time testing may not occur in
accelerated testing
Harsher conditions may result in degradation that
would never occur under normal conditions

Temperature

An increase of 10C from ambient

temperature doubles the rate of reaction
Ambient - 20C
Elevated - 40C stored for 3 months
Equates to 20C for 12 months

Temperature
Alternate Artificial Aging Guides
12 weeks at 45C equates to 24 months
12 weeks at 45C equates to 30 months
16 weeks at 45C equates to 30 months

Guides determined by the Brand /

Manufacturer What do you think is
acceptable?
Where is the intended market?
Elevated temperatures chosen dependant on
product type and ingredients

Temperature
Samples stored at chilled temperature
Control
Used for comparisons

Some samples stored as close to the ambient

market conditions
Assess room temperature stability

Store in dark conditions

Storage conditions must be controlled
Temp control range, fluctuations & variations

Storage temperature monitored daily

Calibrate monitoring equipment regularly
0.5C, 1.0C Incubator / fridge constraints?

Relative Humidity
Immediate packaging test (compatibility)
Does the pack provide adequate protection?
Achieved using saturated salt solutions in a sealed
chamber
Temperature C
Saturated
Solution

10

20

30

40

KNO3

95

93

91

88

NaCL

76

76

75

75

43

42

47
44
Control atKambient
2CO3
Test at humid & dry conditions
Monitor daily

Calibrate monitoring equipment

Cycling / Freeze Thaw

Tests
Fluctuating conditions at regular intervals can
be more stressful than constant conditions
Cycling
Ambient 40C Ambient over 24 hours
Freeze Thaw
-10C 40C -10C over 24 hours

2 week test time

Consider transport / storage conditions
Likely to be more severe than you anticipated

Set temperature controller to cycle between

temperatures

Light
Photostability of product and immediate
packaging
Window light method
Natural daylight North facing
Minimise direct sunlight
Compare to controlled samples kept in dark
condition
Dark incubator
OR; Wrapped in aluminium foil

Consider season and weather variations as it

effects the intensity of light
Not a controlled method

Light
Accelerated light method
Light cabinet SunTest CPS+
Lamp covers whole or broad spectrum of light
e.g. Xenon lamp
Various filters available UV

Utilise cooling system remove effects caused

by temperature
Record data radiant exposure, temperature
and time

Light
Control sample wrapped in aluminium foil
Test sample exposed to light
Test protocols
550W/m2 with C grade filter (window), 2 x 10 hour
exposure (2 tests)
550W/m2 with C grade filter (window), 3 hour to
maximum 12 hour exposure (potentially 4 tests)
550W/m2 with C grade filter (window), 7 x 10 hour
exposure (7 tests)
440W/m2 with C grade filter (window), 20 hour
exposure (1 test)

Test Points
Initial readings
Ensure frequency is sufficient for trends to be recorded
Real Time Stability test PAO
3, 6, 12, 24 & 36 months

Accelerated Stability test 3 month test

2, 4, 8 & 12 weeks

Cycling / Freeze Thaw

1 & 2 weeks

Prior to testing; allow all samples to equilibrate at the

same temperature
Certain tests temperature sensitive
Test under controlled lighting for fair comparison light
cabinet
Suggest 24 hours
Some products may require longer equilibration time

Examination
Physical Stability; common properties
Colour
Appearance
Odour
Assessed subjectively
Multiple assessors to remove bias
Comprehensive description
Rating system to quantify change
Colour
darker / paler
new colours
Appearance
texture
sedimentation
separation
Odour
top / base note
sour / rancid odour developing

Examination
Product specific tests
pH
pH buffers

Viscosity
Calibration fluid

Specific Gravity
Deionised water

Active ingredients
Change in concentration
Interaction with the formulation

Examination
Packaging

Colour
Stress cracking
Tubes rupturing
Panelling / Ballooning
Application Mechanisms
Weight loss / Weight gain
Seal tests

Volume / Pack Number

Requirements
Dependant on

Number of test conditions

Number of test points
Tests required
Product type

Make more than you think you need

Retest the same sample / pack throughout
test?
Simulates consumer usage

OR; test new sample / pack at each test

point?
Simulates product opened for the first time

Interpretation
Product specifications
outside of specification unsatisfactory
reformulate / new pack

Were the specifications too narrow?

Accelerated test
changes observed an accurate prediction of
artificial ageing?
OR; changes due to conditions being too far
removed from the reasonably foreseeable
conditions?

Does the product retain its initial function and

remain safe?
Are the changes aesthetic?