Analytical Methods used for Market Enforcement and Surveillance in the Netherlands

1
Analytical Methods used for Market Enforcement
and Surveillance in the Netherlands
2
Trend

• Emphasis falls on product information enforcement
  (PIF) and less on product examination

3
However

• Product examination is still necessary to check
  at random if the system works well

4
And

• Product examination is necessary to discover
  trends and to initiate product file inspections

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Laboratory

• Accreditation ISO/IEC 170252005
• Chemical and Microbiological team (22 fte)
• 2006 5300 analyses, 2200 for cosmetics (650
  samples tattoo excluded)
• 2007 4200 analyses, 1900 for cosmetics (500
  samples tattoo excluded)
• VIDAS and Anoxomat
• Pathogen laboratory and own preparation of
  culture media
• HPLC (12), GC (5), GC-MS (4), LC-MS, UPLC-MS-MS,
  ICP-MS, FTIR, NIR and XRF

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Microbiological Methods

• Total Count
• Moulds
• Challenge tests
• Enteros
• Pseudomonas
• S. Aureus

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Challenge test

• Pseudomonas aeruginosa, Escherichia coli,
  Staphylococcus aureus, Candida albicans,
  Aspergillus niger
• Test on germ free
• Addition to product of different cultures of
  micro-organisms, yeast and moulds
• After 1 week determination of Total Count
• Addition to product of different cultures of
  micro-organisms, yeast and moulds
• After 1 week determination of Total Count
• Repeat the procedure until no growth is detected
  or until maximal 4 weeks after second addition
• Determination of log reduction

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Challenge test
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Chemical Methods (1)

• Vitamin A, D and E
• Hydrogen peroxide in tooth whiteners
• Local anaesthetics (benzocain, procain, lidocain,
  tetracoin, bupivacain) in creams
• Formaldehyde
• Hydroquinone
• Nitrosamines in shampoo
• Benzisotiazolinone, chloromethylisothiazolinone
  and methylisothiazolinone
• Corticosteroids
• Mercury in soap bars
• Iodopropylbutylcarbamate (IPBC)

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Chemical Methods (2)

• Benzoylperoxide in nail products
• Thioglycolic acid in hair wave products
• Oxidative hair dyes
• Primary aromatic amines in tattoo
• Allergens in perfumes
• Dibutylphthalate and toluene in nail lacquers
• Parabens, phenoxyethanol, benzoic acid, sorbic
  acid and salicylic acid
• Bronopol, Bronidox and methyldibromoglutaronitril
• UV filters
• Ad hoc methods

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Survey Nitrosamines (2004-2007)
SB-Aq 150x4.6 mm, 5 µm Flow 1,0 ml/min Mobile
phase acetic acid (1) and acetonitril
(Gradient) sample extracted with SPE or LLE
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Survey Nitrosamines (2004-2007)
NDELA detected 2004 18 of the samples
(n137) 2005 19 of the samples (n181) 2006 5
of the samples (n394) 2007 4 of the samples
(n668)
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Survey Child Cosmetics (2005-2006)

• Babies/pre-scholars (355 samples) and children gt
  3 years (400 samples)
• Preservatives (parabens, BIT, MI, CMI,
  Formaldehyde)
• Fluoride
• UV filters
• Heavy metals
• Total Count
• Challenge test

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Survey Child Cosmetics (2005-2006)

• Parabens most used preservatives possibly in
  combination with phenoxyethanol
• Presence of benzisotiazolinone (4 out of 137)
• Sodium salt most used form of fluoride
• Presence of NDELA (3 out of 40)
• Ethylhexylmethoxycinnamate, benzophenone-4/5,
  BMDBM and octocrylene most used UV filters in
  products for children lt3 years
• BMDBM and ethylhexylmethoxycinnamate most used UV
  filters in products for children gt3 years
• Presence of Lead (8) and Cadmium (2) (59
  samples)

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Survey Child Cosmetics (2005-2006)

• Total Count gt10 CFU/g is 5 for products for
  children lt3 years (262 samples)
• Total Count gt10 CFU/g is 8 for products for
  children gt3 years (223 samples)
• Challenge test for products for children lt3 years
  were qualified as weak or unsatisfactory (27)
  and at least 2-times unsatisfactory (4)
• Challenge test for products for children gt3 years
  were qualified as weak or unsatisfactory (45)
  and at least 2-times unsatisfactory (6)

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Survey allergens (2006-2007)
CPWax 52CB 50m0.25mm0.20µm sample diluted with
acetone
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Survey allergens (2006-2007)
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(No Transcript)
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Survey allergens (2006-2007)
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Survey Microbiological State (2006)

• 1070 products on water base
• Total Count using Trypton Soya Agar (3 days at
  30C)
• Moulds using Mout Agar (5 days at 25 C)
• Challenge test

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Survey Microbiological State (2006)

• Total Count gt15 CFU/g 4
• Total Count gt1000 CFU/g 1
• Non-compliance challenge test 30
• Shampoo higher Total Count
• Sun care products and creams/ointments score less
  in challenge test
• In most cases the preservative system is not
  adequate for protection against infection of
  moulds

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PAO symbol (2007)

• Statutory requirement for products with shelf
  life gt30 months
• Creams without dispenser system
• Once a week finger-test
• Three weekly microbiological analysis (Total
  Count and Moulds)
• Proceed as long as the product is run out or the
  PAO date is passed
• No results yet

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Conclusion
Product examination is still necessary to
guarantee the safety of use of cosmetics by
consumers.