Stability Testing

The purpose of stability testing is to ensure that the cosmetic product maintains its intended physical, chemical and microbiological quality, as well as functionality and aesthetics when stored under appropriate conditions.

Considerations:

It is up to each manufacturer to determine the appropriate conditions for the use of their products based on knowledge of the formulations and of the intended use, with a focus on:

1. Identify of tests that will “accelerate and predict” the effects of normal conditions of storage and use. Where relevant, consider stresses, including temperature, that will enable assessment of product integrity under anticipated product exposure conditions.

2. Consider evaluation of critical aesthetic properties such as colour, fragrance, texture, and flow, particularly after exposure to conditions designed to stress each specific property.

3. Consider variation in process conditions.

4. Consider the impact of packaging on the contained product, as well as any effects which the product might have on the packaging.

The most common conditions for stability testing of cosmetic products are listed in several published references:

International Federation of Societies of Cosmetic Chemists, IFSCC Monograph, Number 2: The Fundamentals of Stability Testing:

Temperature Humidity Duration
Control 4°C Shelf life
Room Temp 20 – 25° C - Shelf life
Accelerated 37° C - 3-6 months
Accelerated 37° C 80% 1 month
Accelerated 45° C 1-3 months

 

Cosmetic Regulation in a Competitive Environment (Chapter 11; Stability Testing of Cosmetic Products)

Room Temperature: 24-25°C
Accelerated testing: 37, 45 and 50°C
Freeze-thaw cycling: 0 or -5°C
Elevated Humidity: 80% RH

 

Stability testing is an experiment in which samples of the formula are put at different environmental/ storage conditions for a set period of time to simulate what will happen to the product during its life cycle. At selected intervals, samples are evaluated for various physical, chemical and performance characteristics to see if and how they have changed.

1. Selection of batches

  • It is recommended to use at least one batch of the cosmetic product, the same formulation as the marketed product.

2. Container/ Closure system

  • The container/closure system(s) shall be the same as that is proposed for marketing. Any other studies carried out on the cosmetic product outside its immediate container or in other packaging materials can form a useful part of the stress testing of the cosmetic product or can be considered as supporting information, respectively.
  • Appropriate controls (for example, product in glass containers) should be used.

3. Stability evaluation parameters

  • Organoleptical properties: colour, odour and appearance,
  • Physico-chemical properties: pH value, viscosity, density, the monitoring of formulation ingredients (whenever applicable)
  • Microbiological stability: microbial count & Challenge Test of the preserving system made before and/or after the Accelerated Stability Test.
  • Compatibility Test: The compatibility between the content & the container
  • Analytical data in relation to other parameters for specific product type

A good preliminary recommendation is the centrifugation test. This test predicts emulsion creaming for powder and liquid/cream products.

  • A sample heated to 50°C is centrifuged at 3,000rpm for 30 minutes.  For temperature sensitive ingredients the top temperature can be adjusted to 40°C
  • The product must remain stable and any sign of instability shows the need for reformulation.

If the product passes this test, the product can then be submitted for the remaining stability tests.

Preliminary stability test - it is also known as Screening test, Accelerated stability test or Short term test.

  • This test helps screen the formulation in the product development stages
  • The samples are heated, cooled and subjected to alternative heat/cool cycles.

Study duration: 15 days

Parameters evaluated:

  • Organoleptic characteristics: appearance, colour, odour and flavor, whenever applicable.
  • Physical-chemical characteristics: pH value, viscosity, density, or others.

Accelerated Stability Test - also known as normal or exploratory stability test. This test is a predictive study that can be used to estimate the expiry date of the product.

Study duration: 90 days.

Acceptance Criteria

The samples are evaluated in comparison with the standard sample (must remain unchanged during the whole life cycle of the product) and with products that are considered as ‘’references’’ submitted to the same test conditions. Generally limits of acceptance are defined for the evaluated parameters. The interpretation of the data obtained during the Stability Test depends on criteria established in accordance with the formulator’s experience.

Criteria Limits of acceptability
Appearance The product must keep itself entire during the whole of the test, maintaining its initial appearance under all the conditions except high temperatures, freezer conditions or cycles in which small alterations are acceptable.
Colour and odour Must remain stable for at least 15 days when exposed to sunlight. Small alterations are acceptable at high temperatures.
Viscosity The limits of acceptability must be defined by the formulator, considering the visual and sensorial perceptions caused by alterations. The possibility of the consumers also noticing them must be considered.
Compatibility with the containing material The integrity of the package and the formulation must be considered, evaluating the weight, the sealing and the functionality

In cases where the monitoring of the active ingredient percentage is necessary, the quality and performance parameters of the product must be considered.

Other parameters can be established according to the formulator and the products’ specifications.

The Conclusion report on stability study shall contain:

1.  Identification of the product

2. Containing material used in the test

3.  A description of the methodology used to determine the product’s minimum durability. If applicable, the specific preservation precautions should be mentioned.

4.  Study conditions (sample storage conditions, test time period and periodicity of the evaluations). In addition, the following should also be provided:

  • Evidence that the composition of the product used for stability testing corresponds to the product actually placed on the market;
  • The results of the preservative efficacy study, e.g. challenge test, if applicable;
  • When applicable, the period after opening (PAO) and its justification;

5.  The signature of the person responsible for the study