Testing of food contact materials. Viviana Golja, MSc.

Transcription

1 Testing of food contact materials Viviana Golja, MSc.

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

3 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

4 SAMPLING: Representative All FCMs: careful handling and preserving the samples (segregation, protection from light, temperature, moisture, volatiles, test repetition)

5 Plastics

6 Plastics Plastics REGULATION (EU) NO 10/2011 Overall migration Specific migration Examples Prevailing approach Guidance documents

7 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

8 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

9 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).

10 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)

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

12 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

13 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

14 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

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

16 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

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

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

19

20 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!

21 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

22 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.

23 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.

24 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.

25 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

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

27 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 dm 2

28 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

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

30 Overall migration testing worst foreseeable conditions of use in which changes do not take place

31 Overall migration testing all type of foods all types of food except for acidic foods all aqueous + alcoholic foods + milk products all aqueous, acidic and alcoholic foods and milk products all aqueous foods and alcoholic foods up to an alcohol content of 20 % all aqueous + acidic foods + alcoholic foods up to an alcohol content of 20 % distilled water or A + B + D2 distilled water or A + D2 D1 B + D1 C C + B

32 Overall migration testing

33 Overall migration testing

34 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.

35 Overall migration testing

36 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)

37 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

38 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

39 Methods for OM and SM testing total immers. migration cell article filling Specific migration testing more important then overall migration testing

40 Examples Yogurt cup Food simulants B (if ph<4,5) and D1 OM conditions OM1 (10 d at 40ºC) SM conditions - 10 days at 40 C (covers 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). Testing cups by article filling method or plastic sheets by total immersion method; because V cup<0,5l, results of specific migration should use the relation of 6dm 2 /1kg of food.

41 Examples PET bottle for juice (clear drink): Food simulants B (if ph<4,5) and C OM conditions OM2 (10 d at 40 C) SM conditions - 10 days at 60 C (shall cover 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) Testing bottles by article filling method; if V bottle> 0,5L and <10L, results of specific migration shall be expressed in mg/kg applying the real surface to volume ratio in actual or foreseen use, if V bottle <0,5L, results of specific migration should use the relation of 6dm 2 /1kg of food.

42 Examples Plastic plate Food simulants Materials and articles intended for contact with all types of food shall be tested with food simulant A, B and D2. OM conditions OM3 (2 hours at 70 C) SM conditions - Testing for 2 hours at 70 C. Testing plates by article filling method or by total immersion method; if V plate<0,5l, results of specific migration should use the relation of 6dm 2 /1kg of food.

43 Prevailing approach OM testing Results of verification prevail over results of screening SM testing Results in food prevail over results in simulants Results in simulants prevail results over screening

44 Guidance documents Google EURL FCM

45 Ceramics Specific migration of Pb and Cd: 4 % (v/v) acetic acid, in a freshly prepared aqueous solution Test conditions 22 ± 2 C for a duration of 24 ± 0,5 hours.

46 Metals and alloys

47 Metals &alloys: CoE Practical Guide Art. 3 Regulation 1935/2004 Release testing new approach: new simulants envelope volume SRLs

48 Metals &alloys: CoE Practical Guide Release testing into foodstuffs Testing of packaged food Utensils

49 Metals &alloys: CoE Practical Guide Transitional SRLs 0,2 1 0,1 0,6 0,7 0,05

50 Practical Guide Transitional SRLs 0,01 0,05 0,02 0,04 0,015 0,0005

51 Metals &alloys: CoE Practical Guide Envelope volume = X Y Z (in cm3) RW (kg) = Envelope volume (cm3) /1000

52 Metals &alloys: CoE Practical Guide Released mass (M) = V C V: volume of simulant used C: Concentration of the element to be examined in the simulant Determination of the specific release: As a general rule: SR = M/RW

53 Paper and board

54 Paper and board Standards: Paper and board intended to come into contact with foodstuffs Cold water extract EN 645 Hot water extract EN 647 Conditions for migration testing with MPPO EN determination of specific substance or extraction of the material + determination Preparation of an organic solvent extract EN 15519

55 Paper and board Hydrocarbons from mineral oils (Mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) and plastics (Polyolefin oligomeric saturated hydrocarbons (POSH) & Poly alpha Olefine (PAO)) in packaging materials and dry foodstuffs : solid phase extraction + GC-FID

56 Organoleptics testing: Paper and board CEN/TR :2008 CEN/TR :2008 CEN/TR :2008 EN :2010 EN :2010 CEN/TR :2008/AC:2009 CEN/TR :2008/AC:2009

57 Coatings

58 Coatings Art. 3 Regulation 1935/2004 Test conditions according to JRC Guidelines (volontary) CEN/TS 14235: Materials and articles in contact with foodstuffs - Polymeric coatings on metal substrates - Guide to the selection of conditions and test methods for overall migration

59 Conclusion Testing of FCMs is complex and demanding task