Transcript Cosmetics and Sunscreens – Analytical Testing Requirements Scott Colbourne – Business Manager NSW ALS Pharmaceutical Australia RIGHT SOLUTIONS · RIGHT PARTNER.

Cosmetics and Sunscreens –
Analytical Testing Requirements
Scott Colbourne – Business Manager NSW
ALS Pharmaceutical Australia
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Contents
• Australian Regulations – Testing & Stability requirements
• ASEAN
and
EU
Regulations
–
Testing
&
Stability
requirements
• Typical tests - how and why they are performed?
• Why validate / re-validate a method?
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Australian Regulations
• All ingredients in cosmetic products are regulated as
industrial chemicals under the Industrial Chemicals
(Notification and Assessment) Act 1989
• In addition the Cosmetic Standard 2007 covers certain
products
• If a product’s primary function is as a sunscreen it is
regulated by the Therapeutic Goods Administration (TGA)
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Australian Regulations:
Testing of Cosmetics Substances
New chemicals applications via NICNAS* :
•
Spectral data to confirm the structural formula
•
Purity
•
Impurities
•
Additives
•
Valid reproducible physico-chemical data, including:
–
Melting point or boiling point
–
Specific gravity or density
–
Vapour pressure
–
Water solubility
–
Partition coefficient
–
Particle size (distribution) or fibre length
–
Flashpoint, Flammability, Auto-ignition
Information from NICNAS Handbook (Appendix F)
* Not listed on AICS, Australian Inventory of Chemical Substances
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Australian Regulations –
Testing from Cosmetics Standard 2007
• The
Cosmetics
Standard
2007
describes
the
requirements for six cosmetic product categories.
• These categories include various SPF products.
• The only specific testing noted is SPF:
‘product
meets
the
performance
requirements
for
a
broad-spectrum product’
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Australian Regulations – Sunscreens
• TGA regulates as therapeutic goods:
-
Primary sunscreens - SPF 4 or more
-
Moisturisers containing sunscreen with SPF >15
• Sunscreens must comply to ARGS (Australian Regulatory
Guidelines for Sunscreens)
• Efficacy of each sunscreen product is to be tested to
determine the sun protection factor (SPF)
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Australian Regulations – Testing Sunscreens
Stability (ARGS 7.1)
• The data must substantiate the physical, chemical and
microbiological stability of the product for at least the claimed
shelf life
• Stability data is not required to be submitted to the TGA for
product listing
• However may be requested for review by the TGA at any time
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Australian Regulations – Testing Sunscreens
Stability (ARGS 7.1)
• Physical testing (at least): appearance, emulsion stability,
absence of crystallisation, odour, viscosity
• Chemical stability testing (should include): pH, active/s
content.
Using a validated, stability-indicating analytical
procedure (for example, HPLC)
• Microbiological stability - preservative efficacy testing at the
start and end of stability trials
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Australian Regulations – Testing Sunscreens
Stability (ARGS 7.1)
• Accelerated studies require enough time points to allow
statistical analysis as the shelf life is extrapolated
• E.g. 0, (1 or 2), (3 or 4), (5 or 6), 9 and 12 months
• Followed by 24 and 30 months as required
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Australian Regulations – Testing Sunscreens
Quality Control (ARGS 8.2)
•
Where a specific monograph from the pharmacopoeia is available
(BP, Ph Eur or USP-NF), it must be used:
•
This applies to most ingredients – both organic and inorganic
•
In addition many of the excipients (including solvents) used in
sunscreen products are also available
•
Finished products are not the subject of monographs and are
therefore controlled by appropriate “in house” quality control
•
“in house” methods cover identity and relevant physical, chemical
and microbiological properties. Test methods must be validated,
as appropriate.
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ASEAN Cosmetic Directive – Testing Requirements
ARTICLE 9 (Methods of Analysis)
• The following cosmetic product documents shall be
made available to the cosmetic regulatory authority:
– methods used by the manufacturer to check the ingredients
– the criteria used for
• microbiological control of cosmetic products
• chemical purity of ingredients of cosmetic products
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ASEAN Guidelines – Testing Requirements
Appendix
VI
–
ASEAN
Guidelines
for
Cosmetic
Good
Manufacturing Practice
• Raw and packaging material specifications should include:
– Testing parameters and acceptance limits
• Bulk and finished product specifications should include :
– Physical properties
– Chemical assay and/or microbiological assays and their
acceptance
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EU Legislation – Testing Cosmetics
• Legislation is covered under European Union law (1223/2009).
• Each product requires a safety report (Annex I)
• The EU provides a guidelines on Annex I for the cosmetic
product safety report
• Guidelines regarding the testing of cosmetics are taken from
the SCCS (Scientific Committee on Consumer Safety)
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SCCS Notes of Guidance for the EU:
Testing Cosmetics
• Evaluation of new substances includes:
– characterisation and purity of the chemical;
– characterisation of the impurities or accompanying
contaminants;
– solubility;
– partition coefficient (Log Pow);
– additional relevant physical and chemical specifications;
– homogeneity and stability;
– UV-VIS-absorption spectrum
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SCCS Notes of Guidance for the EU:
Testing Cosmetics
Stability and physical & chemical characteristics of the cosmetic product
(4-3.3)
•
The physical stability should be established, ensuring no changes in
physical state during transport, storage or handling of the product.
•
Relevant stability tests
•
Relevant physical and chemical parameters should be controlled for each
batch of the finished product, e.g:
– Organoleptic properties
– pH
– Viscosity
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SCCS Notes of Guidance for the EU:
Testing Cosmetics
Guidelines on Microbiological Quality of the Cosmetic Product (4-4)
•
to ensure the microbial safety of cosmetics for the consumer
•
to maintain the quality and specifications intended of the product
•
Quantitative and qualitative Tests (4-4.2)
– Total viable count
– Pathogens: Pseudomonas aeruginosa, Staphylococcus aureus, Candida
albicans
•
Challenge testing (4-4.3)
– Based on US Pharmacopoeia and European Pharmacopoeia
– The efficacy of the cosmetic product’s preservation through challenge
testing – assessed during product development
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Typical Tests - Physical
•
Appearance
•
Identification
•
Viscosity
•
Density (Specific Gravity)
•
Hydroxyl Value: measure of the content of free hydroxyl groups
•
Peroxide Value: initial evidence of rancidity in unsaturated fats and oils
(primary oxidation)
•
Anisidine Value: also linked to rancidity (secondary oxidation)
•
Saponification Value: how much of the fat will saponify. Can be used as a
measure of average molecular weight
•
pH
•
Acidity/Alkalinity – how much base or acid is required to reach a predetermined pH
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Typical Tests - Chemical
• Sunscreen Raw Materials:
– Tests dictated in Pharmacopoeia Monographs:
- Physical Tests (already covered)
- Assay
- Impurities
• Sunscreen Finished Products:
• Zinc Oxide and Titanium Dioxide – by titration or ICP
• Sunscreen Actives – generally by HPLC
• Preservatives – generally by HPLC
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Typical Tests - Chemical
• Cosmetics and Raw Materials:
– Alcohols
– Fatty acids
– Essential Oils
– Vitamins
– Heavy Metals
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Identification and Assay
to assess:
- Presence
- Purity
- Amount in finished
product
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Typical Tests - Microbiological
•
Initial Consumer Safety, Good Manufacturing Process:
– General
• TAMC
• Yeast and Mould
• Staphylococcus aureus
•
Pathogens
are hygiene
able to
Indicator ofwhich
general
affect
immunocompromised
in water,
environment, raw
users,
wounds,
eyes/ears
materials
and
finished
product
• Pseudomonads
Pseudomonads can affect
appearance – discolouration
and phase separation
Ongoing Consumer Safety – multiple use cosmetics
– Challenge Testing (Preservative Efficacy)
• The test involves inoculating with micro-organisms to challenge
the preservative system
• Generally tested at 2, 7, 14 & 28 days
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Method Validation – what is involved?
• Generally performed for quantitative assays, for actives
and preservatives (e.g. sunscreen raw materials and
finished products)
Linearity
• Linearity / Range
response linear
across the
required range?
Response
– Is the method’s
1800
1600
1400
1200
1000
800
600
400
200
0
y = 200.6379x + 0.0721
R² = 1.0000
0
2
4
6
8
10
Concentration
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Method Validation – what is involved?
• Precision – If I run the method many times
do I get consistent results?
• Accuracy – Do I get the number I am looking
for?
• Specificity – Is there any interference from
another substance?
• Robustness – How does my method cope to
small changes in the parameters?
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Method Validation and Re-Validation – why?
•
As discussed previously – to ensure the result is Accurate, Precise and Specific
•
To satisfy regulatory requirements
Scenario 1: Excipient B is reduced to 45% and Excipient C
increased to 10%
•
A Sunscreen with the following
formulation:
•
–
5% Active A
–
50% Excipient B
–
5% Excipient C
–
40% Excipient D
Probably not, as the ingredients are the same and the
assay should not be affected
Scenario 2: Excipient C is replaced by a new Excipient E
The assay for Active A is validated
Yes, the ingredients are different therefore the new
•
The sunscreen’s formulation is
excipient may:
changed. Is re-validation required?
•
Affect the extraction of the active from the sample
during the method
•
Interfere with the active’s response, giving rise to
specificity issues
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References
• NICNAS Chemical Information - Cosmetics
• Cosmetics Standard 2007 – Australia
• TGA Sunscreens – Regulatory Guidelines
• ASEAN Cosmetics Directive
• European Union law Regulation 1223/2009
• Guidelines on Annex I to Regulation (EC) No 1223/2009
• SCCS'S Notes of Guidance for the Testing of Cosmetic
substances and their safety evaluation - 8th revision
• Draft Guidance for Industry: Cosmetic Good Manufacturing
Practices (US FDA)
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