RIGHT SOLUTIONS · RIGHT PARTNER 1 Cosmetics and Sunscreens – Analytical Testing Requirements Scott Colbourne – Business Manager NSW ALS Pharmaceutical

RIGHT SOLUTIONS · RIGHT PARTNER1

RIGHT SOLUTIONS · RIGHT PARTNER

Cosmetics and Sunscreens – Analytical Testing Requirements

Scott Colbourne – Business Manager NSW

ALS Pharmaceutical Australia


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?


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)


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


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’


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)


Australian Regulations – Testing SunscreensStability (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


• 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




• 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


Australian Regulations – Testing SunscreensQuality 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.


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


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


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)


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



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



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


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 pre-

determined pH


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


Typical Tests - Chemical

• Cosmetics and Raw Materials:

– Alcohols

– Fatty acids

– Essential Oils

– Vitamins

– Heavy Metals

Identification and Assay to assess:

- Presence- Purity- Amount in finished

product


Typical Tests - Microbiological

• Initial Consumer Safety, Good Manufacturing Process:

– General

• TAMC

• Yeast and Mould

• Staphylococcus aureus

• Pseudomonads

Indicator of general hygiene in water, environment, raw materials and finished product

Pathogens which are able to affect immunocompromised users, wounds, eyes/ears

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


Method Validation – what is involved?

• Generally performed for quantitative assays, for actives

and preservatives (e.g. sunscreen raw materials and

finished products)

0 1 2 3 4 5 6 7 8 90

200400600800

10001200140016001800

f(x) = 200.637920168067 x + 0.0721113445378023R² = 0.999995736527028

Linearity

Concentration

Resp

onse

• Linearity / Range

– Is the method’s

response linear

across the

required range?


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?


Method Validation and Re-Validation – why?

Scenario 1: Excipient B is reduced to 45% and Excipient C

increased to 10%

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

Yes, the ingredients are different therefore the new

excipient may:

• Affect the extraction of the active from the sample

during the method

• Interfere with the active’s response, giving rise to

specificity issues

• A Sunscreen with the following

formulation:

– 5% Active A

– 50% Excipient B

– 5% Excipient C

– 40% Excipient D

• The assay for Active A is validated

• The sunscreen’s formulation is

changed. Is re-validation required?

• As discussed previously – to ensure the result is Accurate, Precise and Specific

• To satisfy regulatory requirements


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)

http://www.nicnas.gov.au/chemical-information/cosmetics

http://www.nicnas.gov.au/chemical-information/cosmetics/cosmetics-standard

https://www.tga.gov.au/sunscreens

http://aseancosmetics.org/default/asean-cosmetics-directive/articles-of-acd

http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32009R1223&from=EN

http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32013D0674&from=EN

http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32013D0674&from=EN

http://ec.europa.eu/health/scientific_committees/consumer_safety/docs/sccs_s_006.pdf

http://www.fda.gov/Cosmetics/GuidanceRegulation/GuidanceDocuments/ucm353046.htm#Introduction

