Testing of FCMs – Migration Testing

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Page 1. Testing of food contact materials. Viviana Golja, MSc. ... Specific migration testing: plastics already in contact with food: • Sample preparation. • Analysis ...
Testing of food contact materials

Viviana Golja, MSc.

Overview Testing of: – Plastics – Ceramics – Metalls and alloys – Paper & board – Coatings

Conclusion

FCMs: Regulation 1935/2004 ANNEX I: 1. Active and intelligent materials and articles 2. Adhesives 3. Ceramics 4. Cork 5. Rubbers 6. Glass 7. Ion-exchange resins 8. Metals and alloys 9. Paper and board 10. Plastics 11. Printing inks 12. Regenerated cellulose 13. Silicones 14. Textiles 15. Varnishes and coatings 16. Waxes 17. Wood

All FCMs: SAMPLING: • Representative • careful handling and preserving the samples (segregation, protection from light, temperature, moisture,

volatiles, test repetition)

Plastics

Plastics • Plastics REGULATION (EU) NO 10/2011 – Overall migration – Specific migration – Examples – Prevailing approach

• Guidance documents

Plastics General terms • Overall migration (OM): • total of substances that can migrate (gravimetric analyses) • Measure of inertness • Unit: mg/dm2 (except for FCMs for infants and young children)

• Specific migration (SM): • quantity of one specific substance that migrates • Unit: mg/kg

Plastics Restrictions & specifications • • • •

Overall migration limit (OML) Specific migration limit (SML) Total specific migration limit (SML(T) ) Residual content per food contact surface area (QMA) • Concentration in final product • Specification

Plastics Examples: OML is 10 mg/dm2 (before also 60 mg/kg) SML for formaldehyde is 15 mg/kg QMA for vinyltriethoxysilane: 0,05 mg/dm2

Concentration in final product: phthalic acid, benzyl butyl ester – if technical support agent in concentrations up to 0,1 % in the final product Specification: waxes...high viscosity: …Content of mineral hydrocarbons with carbon number less than 25, not more than 5 % (w/w).

Plastics Separate sets of testing conditions for overall migration and specific migration Revised exposure time and temperature parameters for specific migration testing New simulant = Tenax (for dry foods) Screening tests (extraction, calculation, modelling) and verification test (migration testing)

Plastics Specific migration testing: plastics already in contact with food: • Sample preparation • Analysis of migrated substances • Special cases (e.g. phthalates)

Plastics: compliance testing • PIM Annex V – Testing for specific migration of materials and articles already in contact with food – Testing for specific migration of materials and articles not yet in contact with food – Testing for overall migration – Correction factors applied when comparing migration test results with migration limits

Specific migration testing: plastics not yet in contact with food Verification method: Determination of specific migration (SM) mimicking real migration into food • Use of simulants, t, T, S / V and worst case conditions

Sreening methods – for SM testing and OM testing

Specific migration testing: plastics not yet in contact with food • Contamination before contact? • Sample preparation (instruction for use, DoC?, representative specimen? Only parts intended to come into contact) • Repeated use articles (3 X, substances non detectable and not listed – 1X) • Analysis of migrated substances in simulant • Conventional migration tests

Specific migration testing: plastics not yet in contact with food

Specific migration testing: plastics not yet in contact with food contact with all types of foods: A : Ethanol 10 % B: Acetic acid 3 % D2: Vegetable oil

contact with only dry foods: E: Tenax

If intended only for specific types of foods: Table II in Annex III

Specific migration testing: plastics not yet in contact with food

Specific migration testing: plastics not yet in contact with food

Specific migration testing: plastics not yet in contact with food Specific conditions for contact times above 30 days at room T and below: • accelerated test at elevated temperature: max. 10 days at 60 °C • t and T conditions based on the following formula. • t2 = t1 * Exp ((-Ea/R) * (1/T1-1/T2)) • Calculator!

Specific migration testing: plastics not yet in contact with food Specific conditions for contact times above 30 days at room T and below: 10 days at 20 °C =all storage times at frozen condition 10 days at 40 °C = all storage times at refrigerated and frozen conditions including heating up to 70 °C for up to 2 hours, or heating up to 100 °C for up to 15 minutes

Specific migration testing: plastics not yet in contact with food Specific conditions for contact times above 30 days at room T and below: 10 days at 50 °C = all storage time at refrigerated and frozen conditions including heating up to 70 °C for up to 2 hours, or heating up to 100 °C for up to 15 minutes and storage times of up to 6 months at room temperature 10 days at 60 °C = long term storage above 6 months at room temperature and below including heating up to 70 °C for up to 2 hours, or heating up to 100 °C for up to 15 minutes.

Specific migration testing: plastics not yet in contact with food • Specific conditions for contact times above 30 days at room T and below: • storage at room temperature = 10 days at 40 °C if there is scientific evidence that migration of the respective substance in the polymer has reached equilibration under this test condition.

Specific migration testing: plastics not yet in contact with food Specific conditions for combinations of contact times and temperature: - different combinations of contact time and temperature the testing = test conditions which are recognised to be the most severe - if successively subject to a combination of two or more times and temperatures = successively to all the applicable worst foreseeable conditions using the same portion of food simulant.

Specific migration testing: plastics not yet in contact with food

• Repeated use articles • • 3 X - third test result for compliance • • First test when proof of no increase and compliant • • First test when SML = ND and for non listed substances used behind FB

Specific migration testing: plastics not yet in contact with food Analysis of migrated substances

Specific migration testing: plastics not yet in contact with food • Residual content per surface area QMA

• For substances unstable in food simulant or food or for which no adequate analytical method available = residual content per 6 dm2

Specific migration testing: plastics not yet in contact with food SCREENING

• Replacing specific migration by overall migration • (only for non-volatile substannces) • Residual content (calculation of migration potential) • Migration modelling • Food simulant substitutes

Specific migration testing: plastics not yet in contact with food Standardised test conditions: • 7 standard testing conditions • 2 alternative test conditions (high temperature)

Overall migration testing

•worst foreseeable conditions of use in which changes do not take place

Overall migration testing all type of foods all types of food except for acidic foods all aqueous + alcoholic foods + milk products

distilled water or A + B + D2 distilled water or A + D2 D1

all aqueous, acidic and alcoholic foods and milk products

B + D1

all aqueous foods and alcoholic foods up to an alcohol content of 20 %

C

all aqueous + acidic foods + alcoholic foods up to an alcohol content of 20 %

C+B

Overall migration testing

Overall migration testing

Overall migration testing • Substitute test for OM7 with food simulant D2 • If technically not feasible to perform OM7 with food simulant D2 OM 8 or OM9 can be used with a new test sample.

Overall migration testing

Overall migration testing

• Repeated use articles contact – 3 X • Compliance testing= level of the migration found in the third test (if level is not increased and not exceeded in first test)

Overall migration testing SCREENING: More severe than the verification method: • Residual content (Calculation based on the residual content of migratable substances determined in a complete extraction of the material or article) • Use of food simulant substitutes

Overall migration testing • Correction of migration into food simulant D2 • For some food categories migration test result into food simulant D2 shall be divided by written figure before comparing with the migration limit 10 mg/dm2

Methods for OM and SM testing

total immers.

migration cell

article filling

• Specific migration testing – more important then overall migration testing

Examples • Yogurt cup – Food simulants – B (if pH

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