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17/11/2010 FSAI FCMs Seminar, Morrison Hotel, 16 November 2010 1 Food Contact Materials: Use and Control Testing of Food Contact Materials John Keegan Public Analyst’s Laboratory Dublin

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17/11/2010 FSAI FCMs Seminar, Morrison Hotel, 16 November 2010

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Food Contact Materials:Use and Control

Testing of Food Contact MaterialsJohn Keegan

Public Analyst’s LaboratoryDublin

17/11/2010 FSAI FCMs Seminar, Morrison Hotel, 16 November 2010

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Overview• Background on Public Analyst’s Laboratories

• EURL–NRL Network

• E.F.S.A. and E.U. Legislation

• Laboratory testing

• Useful Links

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Public Analyst Laboratories

• There are three–Dublin, Cork, Galway• Analyse all Food of Non-animal Origin• Also Food Contact Materials (FCMs)• Dublin is the specialist laboratory for FCMs• Accredited to ISO 17025 Standard• Service Contract with FSAI• Work with Environmental Health Service• Together develop an Annual National Food

Sampling Programme (incl. FCMs)• Report non-conformances to EHS and FSAI

17/11/2010 FSAI FCMs Seminar, Morrison Hotel, 16 November 2010

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EURL–NRL Network• Regulation 882/2004–Article 32 provides for

European Union Reference Laboratory (EURL) for many areas of official controls on food, including FCM

• Article 33 obliges each Member State to appoint a National Reference Laboratory (NRL) in each area

• Public Analyst’s Laboratory, Dublin appointed in 2006 as NRL for FCMs

• These Articles also define the functions of both the EURL and NRL laboratories

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Functions of EURL (1)1. Providing NRLs with details of analytical methods,

including reference methods

2. Co-ordinating application by NRLs of the methods, in particular by organising comparative testing and by ensuring an appropriate follow-up of such comparative testing in accordance with internationally accepted protocols

3. Co-ordinating practical arrangements needed to apply new analytical methods and informing NRLs of advances in this field

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Functions of EURL (2)4. Conducting initial and further training courses for the

benefit of staff from NRLs and of experts from developing countries (incl. potential new Member States)

5. Providing scientific and technical assistance to the Commission, especially in cases where Member States contest the results of analysis

6. Collaborating with laboratories responsible for analysing feed and food in Third Countries

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Functions of NRL• Useful source of expertise to CA• Disseminate information to Official Control

Laboratories (OCLs)• Evaluating laboratory results• Dealing with conflicting results• Method development• Performance testing (Ring trials)

– To participate in them– To organise them for other OCLs

• Dublin is both an NRL and an Official Control Laboratory

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Legislation

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Rapid Alert System• The Rapid Alert System for Food and Feed

(RASFF)• Put in place to provide food and feed control

authorities with an effective tool to exchange information about measures taken responding to serious risks detected in relation to food or feed

• This exchange of information helps Member States to act more rapidly and in a coordinated manner in response to a health threat caused by food or feed

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RASFF Notifications 2010

• Heavy metals in ceramics (e.g. Pb, Cd, Cr, Ni)• Formaldehyde in melamine kitchenware• Primary aromatic amines in black nylon kitchen

utensils• Overall migration problems• Photoinitiators• Phthalates (plasticisers)• Melamine (1)• Semicarbazide (1)• Miscellaneous

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History of FCM testing at PALD

• 2002–BADGE/BFDGE• 2003–BADGE/BFDGE, SEM• 2004–BADGE/BFDGE, SEM, ESBO• 2005–SEM, ESBO, 2-EHA• 2006–BADGE, SEM, ESBO, 2-EHA, ITX• 2007–SEM, ESBO, ITX• 2008–ESBO, PAAs, Phthalates, Adipates,

Sebacates• 2009–ESBO, PAAs, Phthalates, Adipates,

Sebacates, Melamine

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Current testing

• 2010–ESBO, PAAs, Phthalates, Melamine, Formaldehyde, Lead and Cadmium, Bisphenol A

• 2011–ESBO, PAAs, Phthalates, Melamine, Formaldehyde, Lead and Cadmium, Bisphenol A, Nickel and Chromium, Photoinitiators

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Irish Sample Numbers

2009 2010PAA 16 40

Formaldehyde n/a 20

Melamine 20 20

Phthalates 45 30

Ceramics 60 60

ESBO 45 30

Bisphenol A n/a 50

Total 186 250

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Key point

• Official control sampling is not a replacement for industry own-checks as part of their responsibility under Regulation 1935/2004 and the specific measures

• Look for the symbol

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Testing of FCMs

• Several possibilities– Test migration from articles using food

simulants– Test packaged food to see if migration has

taken place– Test foods with packaging under controlled

conditions to determine if migration takes place

– Migration modelling

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Testing of FCMs

• Guidelines on Testing Conditions for Articles in Contact with Foodstuffs (http://crl-fcm.jrc.it/files/guidelines%20test%20conditions_final_ed2009.pdf )

• Guidelines for Performance Criteria and Validation Procedures of Analytical Methods used in control of Food Contact Materials (http://crl-fcm.jrc.it/files/Method_Perf_Guidelines_final_ed2009.pdf )

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Test conditions

Food type SimulantAqueous food (pH > 4.5)

Distilled water A

Acidic foods (pH ≤ 4.5)

Acetic acid 3% in water (w/v) B

Alcoholic foods Ethanol 10% in water (v/v)(adjust % for foods with >10%)

C

Fatty foods Rectified olive oil or other fatty food simulants

D

Dry foods None (Tenax)

Milk products Ethanol 50% in water (v/v)

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Test Methods (1)

• EN series:• 1186 (Overall Migration for Plastics)–15 parts

• 13130 (Specific Migration for Plastics)–28 parts– (http://www.standards.ie/ )

• EURL compendium of analytical methods (450):– (http://crl-fcm.jrc.it/resource_centre/smm.php )

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Test Methods (2)

• One-sided migration test for multi-layer materials in the lid of the cell

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Example (1)

• Black Nylon kitchen utensils (PAAs)

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Example (2)

Qualitative analysis:

for nylon by FT-IR

Sample preparation:•Immerse theoretical cooking surface in 3% acetic acid•Boil for 2 hours•Repeat boiling three times

Quantitative analysis:•Final volume is recorded•Extract injected onto LC-MS/MS

Calculations

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Example (3)

• Analyse 3% acetic acid solutions• Calculate surface area of contact with food• Calculate specific migration• Results expressed as µg/dm2 or µg/kg • Check against legislation for conformance

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Example (4)

• Surface area calculation– Break down into constituent parts– Get the surface areas of the constituent parts– Sum the surface areas– Obtain the total surface area

• Websites for surface area calculations– http://www.analyzemath.com/Geometry_calculators/

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Analytical Techniques

• FT-IR–identify plastic materials• HPLC with UV, fluorescence detection etc.• UPLC-MS/MS analysis• GC-MS analysis• ICP-MS (for metals)• Overall migration (gravimetric)• Non-targeted Mass Spec analysis

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Useful links!• http://ec.europa.eu/food/food/chemicalsafety/foodcontact/legisl_list_

en.htm (Legislation tree)

• http://eur-lex.europa.eu/en/index.htm (EU law)• http://ec.europa.eu/food/food/rapidalert/index_en.htm (RASFF)• http://www.akts.com/ (Migration modelling)• http://www.fabes-online.de/profil.php?lang=en (migration

modelling and migration cell)• http://modmol.agroparistech.fr/sfpp3/SFPP3_quick_start/ (Migration

modelling)• Plastic Packaging: Interactions with Food and Pharmaceuticals, 2nd

Edition, Otto Piringer and Albert Baner, Wiley-VCH Verlag GmbH

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Acknowledgements

• Food Safety Authority of Ireland

• Dr Bernard Hegarty, FSAI

• Eimear McCall, Post-grad. Student

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Sir Patrick Dun’s