Professional Documents
Culture Documents
Testing
Presented by
Ian Lyle (Port Sunlight)
Chadaporn Kusumarn (Shanghai)
Topics to be covered
Data recording
Topics to be covered
Data recording
Stability – Why Bother?
World class brands are built on world class quality products.
Data recording
Stability Testing
Our Stability Protocols are broken down into two main
categories of testing:
The FDA in the USA bases their guidelines for Drug Expiration Dating on
the ICH Guidelines. The temperatures cited in the ICH Guidelines are
based primarily on a Global Climate Survey conducted by W. Grimm which
was an extensive study that included warehouse temperatures, extremes,
average temps and the number of days particular cities in various regions
were above the Mean Kinetic Temperature.
Since 45C covers the worst case scenario for Long Term Product Stability
Testing and is in wide use throughout Unilever, the range suggested in the
COLIPA , IFSCC and ICH Guidelines are reasonable to recommend.
Stability of a Cosmetic Product
INITIAL P,C,M
1 Week P,C
4 weeks P P,C P,C,M
8 weeks P P,C P,C
12 weeks P P,C,M P P,C
13 Weeks for OTC
Sample Requirements:
Some attributes such as pH, viscosity and micro have well defined numerical
specification ranges, but others are more vague (“compare with standard”)
Currently there are no fixed standards for what are acceptable and unacceptable
changes in physical characteristics – it is up to the judgment of individual
formulators.
Category workshop planned in 2007 to begin to define common reference points
for these
Example: SE Asia Grading Scale
1) Sign of Separation
SCORE DESCRIPTION
0 OK
1 10% Cracking in shampoo texture
2 20% Cracking in shampoo texture
3 30% Cracking in shampoo texture
4 40% Cracking in shampoo texture
5 50% Cracking in shampoo texture or more
2) Phase Separation
SCORE DESCRIPTION
0 OK
1 0.1 cm. of transparent level on top
2 0.2 cm. of transparent level on top
3 0.3 cm. of transparent level on top
4 0.4 cm. of transparent level on top
5 0.5 cm. of transparent level on top or more
Signs of Physical Instability
Shampoo samples scored according to SE Asia scale:
Sign = 1 Sign = 2
Sep = 1 Sep. = 2
Sign = 3 Sign = 4
Sep = 4 Sep = 3
When to do stability testing
Stability testing of the formulation (CUC) should be started as
soon as possible during product development, even if the full
formulation is not yet defined. This should allow early
identification of any fundamental issues that need to be
resolved as part of the product development process.
1. 2. 3. 4. 5.
Project Brief - Charter Concept Design Specification
Technical -Technical Lock Lock Lock
Section section
Lab/Pilot Full scale
scale manufacture
stability stability
proven proven
At Spec lock – final stability must be complete (full scale manufacture product
in final pack) with final ingredient and product specifications in InterSpec
Topics to be covered
Data recording
Factors affecting stability
Ingredient chemistry
New ingredient (or more often a sub-component or impurity)
Specification definition
Inadequate processing
e.g. incomplete hydration of polymers such as Jaguar and Carbopol
can lead to increasing viscosity over time
Hydrolysis of ingredients
e.g. DLSS hydrolysis leads to production of laureth-3 which
increases viscosity
Change in fragrance
Fault in packaging
e.g. pinholes in aerosol can lining leading to corrosion
New packaging (material and colour)
Sunlight (for transparent packs)
Formulation Chemistry
e.g. Dove shampoo formulation
DI Water
Carbopol Slurry (2%)
In order to solve any SLES-1 (25%)
instability problems with your Guar C13S
Sodium Hydroxide (50%) What are the emulsifiers
formulation it is critical that used in the silicone emulsion?
you understand the basic DLSS (32%)
What else is in Euperlan, apart
chemistry associated with the Glycerin from EGDS?
Polyox WSR 308 How might these additives
key ingredients.
Methocel 40-202 affect stability of the product?
CAPB (28%)
By understanding the Euperlan KE 3795
potential interactions between (Euperlan KE 3795 contains
Si macro emulsion SLES-1EO and CAPB)
ingredients you can begin to Tetrasodium EDTA (39%)
generate technical hypotheses Fragrance
for the cause of the instability. Kathon CG
DMDM Hydontoin
Sodium Chloride (20%)
PPG-9
OH
O OH
O O
OSO3Na
O
O OH
OH OH
O n=3-12
n
Ethylene Oxide
It is a cocktail of a mixture of small OSO 3Na of n=3-12
amounts
O Sulphur Trioxide
a variety of residual feedstock and by-products
n NaOH
OH
O O
O OSO3Na
O
O OH
OSO3Na n=3-12
O
OH n=3-12 n
O
n
Non-ethoxylated material
Sulphur Trioxide Distribution of EO units
NaOH
Unsulphated material Distribution of alkyl chain lengths
+ NaCl? OSO3NaCitric acid? NaSO4?
Pack & Fragrance Interactions
Simple changes in packaging &
fragrance can lead to changes in
Product stable in stability e.g. colour and odour
glass container
Effect of
change in Effect of
plastic change in
composition plastic dye
Data recording
Sunsilk Volume Combing Cream
● New Sunsilk Volume range launched in Europe Jan 2004 (Project
Einstein); combing cream had “ultra low fat” conditioner base with
performance superior to Kerastase.
● Storage testing done on samples from lab and pilot scale production;
no main plant trial done.
● Crisis Team formed to find resolve issue and minimise launch delay
14000
12000
10000
İS
.V
8000
6000
4000
2000
DAY
Stability problem
Significant increase in viscosity of shampoos with
6/4/3 surfactant base over time at high storage
temperatures
Hydrolysis of DLSS in 6/4/3
O
R [O CH2CH2 ] O
n R [O CH2CH2 ] OH
ONa n
O SO3 Na +
O
HO
ONa
O SO3 Na
Loss of DLSS
16000
14000
12000
Viscosity (cP) ))
10000
8000
6000
2.2 wt% NH4Cl
4000
0.2 wt% NH4Cl
2000
0
0 1 2 3 4 5
o
Weeks at 49 C
Data recording
Data Recording
Contact:
Rob Waight (Ext. 3219)
FReg and Stability Testing
What are we doing now?
Links to FReg:
Formulations
Ingredients
Equipment