Enlargement and Integration Workshop

Transcription

1 Enlargement and Integration Workshop EU legislation and testing for the chemical testing of food contact materials Ispra, 6-7 November 2012 C. Simoneau, E. Hoekstra, N. Jakubowska 2012 Report EUR 25599EN 1

2 European Commission Joint Research Centre Institute for Health and Consumer Protection Contact information Catherine Simoneau Address: Joint Research Centre, Via Enrico Fermi 2749, TP 260, Ispra (VA), Italy Tel.: Fax: This publication is a Reference Report by the Joint Research Centre of the European Commission. Legal Notice Neither the European Commission nor any person acting on behalf of the Commission is responsible for the use which might be made of this publication. Europe Direct is a service to help you find answers to your questions about the European Union Freephone number (*): (*) Certain mobile telephone operators do not allow access to numbers or these calls may be billed. A great deal of additional information on the European Union is available on the Internet. It can be accessed through the Europa server JRC76765 EUR EN ISBN (pdf) ISSN (online) doi: /67212 Luxembourg: Publications Office of the European Union, 2012 European Union, 2012 Reproduction is authorised provided the source is acknowledged. Printed in Italy 2

3 Executive Summary In the framework of the "Enlargement and Integration initiative", the European Commission Joint Research Centre (JRC) organised a training workshop focusing the latest EU Directives and legislative requirements for food contact materials (FCM), and details of the experimental procedures for compliance testing against the requirements. The training was conceived by the operating manager of the EURL FCM C. Simoneau. The programme included lectures and test demonstrations by C, Simoneau, E. Hoekstra, and N. Jakubowska. The workshop took place in Ispra on 6 7 November The list of topics covered included: EU Directives and legislative requirements for FCM including active and intelligent materials, requirements for compliance for imports, Testing for compliance for plastics including modelling as well as for materials other than plastics, testing specific migration for dry foods with the new simulant in the newly established Regulation 10/2011, and method validation, requirements for quality assurance and proficiency testing programmes. This training also included a laboratory visit and was the subject of a satisfaction survey. The outlook of the training showed a significant impact for the participants not just as shown by the satisfaction survey but also by the spontaneous e mails also received as follow up. The feedback of the training also showed the necessity and wishes for further trainings and collaborations in this field. 3

4 Table of contents Executive Summary...3 Table of contents...4 Programme...5 Presentations...6 Lecture 1: Introduction to food contact materials...6 Lecture 2: EU Directives and legislative requirements for FCM Lecture 3: Procedure and testing requirements for importing FCM in the EU Lecture 4: Active and intelligent packaging Lecture 5: Testing compliance: migration testing for plastics Lecture 6: Migration modelling for compliance testing of plastic FCM Lecture 7: Correction factors of experimentally determined specific migration 113 Lecture 8: Testing compliance for materials other than plastics Lecture 9: Testing for dry foods tests with the new simulant Lecture 10: Method validation requirement and quality assurance plans Satisfaction survey and customer feedback Annex 1 Highlights photos from the training Annex 2 Participants Annex 3 Customer satisfaction survey

5 Programme Workshop "EU legislation and testing for the chemical safety of food contact material" Updated AGENDA /11/ :30 transport to JRC 28F 09:00 09:30 Introduction (C. Simoneau) 09:30 10:30 EU Directives and legislative requirements for FCM (E. Hoekstra) Coffee 11:00 11:30 Requirements for compliance for imports (C. Simoneau) 11:30 12:00 Active and Intelligent materials (E. Hoekstra) 12:00 13:00 Testing for compliance for plastics (C. Simoneau) Lunch 14:30 15:00 Migration modelling (E. Hoekstra) 15:00 15:30 The use of reduction factors for plastics (E. Hoekstra) 15:30 15:45 Compliance: expression of results (E. Hoekstra) Coffee 16:15 17:15 Testing compliance for materials other than plastics (C. Simoneau) Q&A 17:30 transport to hotel 07/11/ :00 Transport to JRC 28F 09:00 10:00 Testing for dry foods tests with the new simulant Tenax (N. Jakubowska) 10:00 10:30 Method validation (C. Simoneau) Coffee 11:00 11:30 Reference materials and proficiency testing programmes (C. Simoneau) 11:30 12:30 Lab visit overall migration (immersion, cells), testing with Tenax 12:30 14:00 Lunch 14:00 15:00 Testing kitchenware and worked examples (C. Simoneau) Q&A, wrap up session ±16:00 closure (depending on travel schemes) 5

6 Presentations Lecture 1: Introduction to food contact materials Slide 1 Institute for Health and Consumer Protection Science for a healthier life Slide 2 Introduction to Food Contact Materials Catherine Simoneau 6

7 Slide 3 Food contact materials Food processing Packaging equipment, tubing, conveyor belts, materials etc Kitchenware, utensils, etc Slide 4 General food law High protection of human health Effective functioning of internal market Food safety: unsafe food = detrimental to health unfit for consumption (contaminated) Law: EC 178/2002 7

8 Slide 5 Package INTERACTION Foods Slide 6 Safety in development and innovation Innovation to assure quality of food and to extend its shelflife Interest of all official institutions New materials (production and design) Materials and containers with specific technical characteristics Development of control techniques to assure quality and safety of packaged food 8

9 Slide 7 Importance of packaging Packaging is beneficial Protects foodstuff from spoilage However the transfer of chemicals from packaging to food may have a negative impact on the quality and safety of the food No food contact material is completely inert Need to ensure the safety of these materials Slide 8 Contamination from food packaging Prolonged contact between food and non-food material Possibility that ingredients from the packaging could be transferred into the food = migration 9

10 Slide 9 Types of food packaging materials Conventional: Plastics, Regenerated cellulose, Paper and board, Glass and ceramics, Elastomers, Metals, Wood, textile, waxes etc. Recycled Biobased: made from renewable sources Active: acts on atmosphere inside package Intelligent: indicators that follow quality during shelf life Slide 10 What is migration? The mass transfer from an external source into food by submicroscopic processes May impact food in two ways Food safety migration of harmful substances Food quality migration of substances which impart taint or odour Packaging Migration Food 10

11 Slide 11 Factors affecting migration Migration is a diffusion and partitioning process that is dependent on: The nature of the food contact material (FCM) The nature and concentration of the migrating substance The nature of the foodstuff The nature, the extent and the type of contact between the food contact material/article and the foodstuff Slide 12 The nature of the FCM Depiction of chemical migration from an impermeable material Packaging Food Impermeable materials: - glass & ceramics - metals & alloys x y z 11

12 Slide 13 The nature of the FCM Depiction of chemical migration from a permeable material Packaging Food Permeable materials: -plastics - rubber & silicone - coatings x y z Slide 14 The nature of the FCM Depiction of chemical migration from a porous material Packaging Food Porous materials: e.g. paper and board y x z 12

13 Slide 15 The nature of the substance Ingredients needed to make plastics Monomers and starting substances Catalysts Solvents and suspension media Additives Antioxidants, antistatics, antifogging, slip additives, plasticisers, heat stabilisers, nucleating agents, dyes and pigments Slide 16 Typical additives for plastics Stabilisers UV absorbers Preservatives Optical brighteners Foaming agents Release agents etc Anti-oxidants Plasticisers Lubricants Emulsifiers Fillers Flame retardants Impact modifiers M.P Steven, Journal of Chemical Education, 1993,

14 Slide 17 Potential migrants from plastics Bis(2-ethylhexyl) phthalate = DEHP Bis(2-ethylhexyl) adipate = DEHA Irganox 1330 BHT Irganox 1076 Irganox 1010 Acetyl tributyl citrate = ATBC Chimassorb 81 plasticisers (up to 40%) antioxidants (up to 0.5%) Slide 18 The nature of the migrating substance Migration into food (mg/kg) Da additive 500 Da additive 1000 Da additive Time (days) 14

15 Slide 19 The nature of the foodstuff Migration (mg/dm 2 ) no fat 10% fat 20% fat 30% fat 50% fat Low fat = high caprolactam migration 0.5 High fat = low caprolactam migration Time (days) Slide 20 The nature of the contact Interaction between food and packaging Direct versus indirect contact Point or continuous contact 15

16 Slide 21 Time and temperature MIgration (mg/kg) C 30 C 40 C Time (days) Slide 22 Potential migrants from printing inks Binders (monomers) Colourants and pigments Solvents to dissolve pigments and resins Catalysts or initiators of UV curing 16

17 Slide 23 Potential migrants from paper and board INGREDIENTS Chlorine bleaches Sizing agents derivatives (strength of paper when wet) Fat repellents Volatiles SUBSTANCES MIGRATING chlorophenols formation waxes, starch fluoroalkyl polymers aldehydes, ketones Slide 24 Potential migrants from (coated) metal Lacquers Tin Epoxy and epoxy-phenolics BADGE, BFDGE from the epoxy resin hydroxy and chlorinated derivates Vinyl systems vinyl chloride and vinyl acetate Tinplate for cans Tin, chromium 17

18 Slide 25 Potential migrants from recycled FCMs Incomplete cleaning of substrate Mis-use of FCMs entering into the recycled food packaging stream e.g. detergents, industrial chemicals Non-FCM materials and articles entering into the recycled food packaging stream e.g. newspaper and magazine print Slide 26 Safety of food contact materials Prevent migration of chemicals to food in unsafe levels Allow use of substances (toxicological data) Impose limits of migration Overall migration + Specific migration for each substance Testing: need of (harmonised) methods Number of substances (> 3000) and materials Testing = migration & (identification quantification) 18

19 Slide 27 Food contact safety: who does what? Risk assessment: European Food Safety Authority (EFSA) Risk management: Commission DG Health and Consumer Protection (SANCO), Enforcement: Member States Slide 28 Food contact safety: who does what? Monitoring and inspection: National Official Control Laboratories supported by National Reference Laboratories Scientific support: European Union Reference Laboratory (JRC) Regulation OFFC EC/882/2004 supported by Network of NRLs 19

20 Slide 29 Remarks Consumers demand High food quality maintained by packaging (active too) Convenience by packaging (resealable, monoportions etc) Food protection by packaging (product integrity) Packaging technology must respond to needs Barrier to bioterrorism (integrity, intelligent) Waste reduction: 3Rs (recyclability, biobased) Information carrier (labelling); traceability Slide 30 Remarks Packaging technology must also: Not be a source of contamination to the food Role of legislation, risk assessment and monitoring enforcement: The inspections are crucial The laboratories are crucial 20

21 Slide 31 Seminar programme 1. EU Directives and legislative requirements for FCM; 2. Framework of implementation of the EU legislation on FCM; 3. Active and intelligent materials 4. Compliance testing for plastics overall and specific migrations ) Slide 32 Seminar programme 5. Method validation and verification for testing procedures for compliance testing; 7. Reference materials and proficiency testing programmes; 8. Kitchenware and worked examples 21

22 Slide 33 The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States 22

23 Lecture 2: EU Directives and legislative requirements for FCM Slide 1 EU Directives and legislative requirements for food contact materials Eddo J. Hoekstra Joint Research Centre The European Commission s in-house science service Slide 2 EU legislation on food contact materials 23

24 Slide 3 Overview Introduction and general principles EC legislation of Food Contact Materials (FCMs) Other legal or recommended provisions in the EU Framework of implementation of EU legislation on FCM Slide 4 Who does what Risk management European Commission (DG SANCO) Risk assessment + sampling advice European Food Safety Authority (EFSA) Official control MS competent authorities High quality and uniformity of analytical results European Union Reference Laboratory for FCM (EU-RL) Food and Veterinarian Office (FVO) Other European organisations Council of Europe (CoE) European Standardisation Organisation (CEN) 24

25 Slide 5 European Union Croatia Slide 6 How and when did it all start? Vinyl chloride monomer (VCM) 1972 cause of liver cancer in laboratory animals 1973 migration from PVC food packaging materials 1973 MAFF WG on VCM was established 1974 Clear link between angiosarcoma and occupational exposure of US workers 1978 Directive 78/142/EEC sets QM = 1 mg/kg and SML=ND (0.01 mg/kg) 25

26 Slide 7 EU legislation Food contact materials (EC) No 1935/2004 Good manufacturing practice (EC) No 2023/2006 Regenerated cellulose film 2007/42/EC Ceramics 84/500/EEC as amended Plastics Active and intelligent materials (EC) No 450/ Coatings Elastomers and rubbers Vinyl chloride 78/142/EEC 80/766/EEC 81/432/EEC Monomers and additives 2002/72/EC as amended Plasticisers in gaskets (EC) No 372/2007 as amended Migration testing 82/711/EEC as amended List of simulants 85/572/EEC as amended Recycled plastics (EC) No 282/2008 BADGE/BFDGE/ NOGE 1895/2005/EC 93/11/EEC Nitrosamines Reproduced with the kind permission of Annette Schaefer (DG-SANCO, European Commission) Slide 8 EU legislation Food contact materials (EC) No 1935/2004 Good manufacturing practice (EC) No 2023/2006 Regenerated cellulose film 2007/42/EC Ceramics 84/500/EEC as amended Plastics Active and intelligent materials (EC) No 450/ Coatings Elastomers and rubbers Vinyl chloride 78/142/EEC 80/766/EEC 81/432/EEC Monomers and additives 2002/72/EC as amended (EU) No 10/2011 Plasticisers in gaskets (EC) No 372/2007 as amended Migration testing 82/711/EEC as amended List of simulants 85/572/EEC as amended Recycled plastics (EC) No 282/2008 BADGE/BFDGE/ NOGE 1895/2005/EC 93/11/EEC Nitrosamines Reproduced with the kind permission of Annette Schaefer (DG-SANCO, European Commission) 26

27 Slide 9 Framework Regulation (EC) No 1935/2004 Food contact materials First step to harmonising legislation Defines what is meant by food contact materials and articles Two general principles Inertness Safety Slide 10 Framework Regulation scope Materials and articles in contact with food intended for food contact expected to come into NOT contact with food Antiques Covering/coating materials that form part of the food and Use of materials for are consumed with the food Food packaging Fixed public or private water Kitchen articles supply equipment Machines or articles used for food manufacture and processing 27

28 Slide 11 Framework Regulation Article 3 Materials and articles, including active and intelligent materials and articles, shall be manufactured in compliance with good manufacturing practice so that, under normal or foreseeable conditions of use, they do not transfer their constituents to food in quantities which could: a) endanger human health b) bring about an unacceptable change in the composition of the food c) bring about a deterioration in the organoleptic characteristics thereof Slide 12 Framework Regulation specific measures Empowers the Commission to set requirements, e.g. a list of substances authorised for use in the manufacturing of materials or restrictions, for specific materials or substances: 1) Active and intelligent 9) Paper and board materials and articles 10) Plastics 2) Adhesives 11) Printing inks 3) Ceramics 12) Regenerated cellulose 4) Cork 13) Silicones 5) Rubbers 14) Textiles 6) Glass 15) Varnishes and coatings 7) Ion-exchange resins 16) Waxes 8) Metals and alloys 17) Wood 28

29 Slide 13 Framework Regulation role of EFSA Any provision which may affect public health shall be adopted after consulting the European Food Safety Authority (EFSA) When there is a positive list any substances included in this list should first be evaluated by EFSA Procedure: manufacturer MS competent authority EFSA Other MS CA Standing Committee on the Food Chain and Animal Health (SCFCAH) EC + Comitology Authorisation Slide 14 EU conventions for SML The EU SML are based on toxicology and exposure SML (mg/kg food) = NOEL (mg/kg bw) 60 kg bw / 1 kg food However, pending a best estimation of exposure, the EU system is based in migration assuming that: 1 person of 60 kg ingest daily 1 kg of food in contact with 6 dm 2 of surface containing the substance at the maximum concentration permitted (SML) 29

30 Slide 15 Framework Regulation labelling If an article is intended for food contact it shall be labelled with: for food contact or a specific indication as to their use or the FCM symbol and If necessary, special instructions to be observed for safe and appropriate use and Name and address manufacturer and Traceability details Not obligatory where the intention for food contact is obvious by the nature of the article e.g. knife, fork, wine glass Slide 16 Framework Regulation labelling Labelling, advertising and presentation of food contact materials shall not mislead the consumer At the retail stage, the labelling information shall be displayed on: the materials and articles or on their packaging or labels affixed to the materials or to their packaging or a notice in the immediate vicinity of the materials and articles and clearly visible to purchasers 30

31 Slide 17 Framework Regulation DoC Declaration of compliance (DoC) Materials and articles shall be accompanied by a written declaration stating that they comply with the rules applicable to them Appropriate supporting documentation shall be made available to the enforcement authorities to demonstrate such compliance Slide 18 Framework Regulation traceability Traceability = ability to trace and follow a material or article through all stages of manufacture, processing and distribution The traceability of the material or article shall be ensured at all stages in order to facilitate: control the recall of defective products consumer information the attribution of responsibility One step forward & one step back 31

32 Slide 19 Regulation (EC) No 2023/2006 Good Manufacturing Practice (GMP) Addressed to business operators Article 3 of Framework Regulation requires GMP ensuring safety and inertness Minimum requirements Annex on application of printing inks and storage of printed materials Slide 20 GMP minimum requirements Establish, implement and maintain a quality assurance system Adequacy of processes design and operation Adequacy of premises and equipment Adequacy of raw materials selection and specification Established operation procedures and instructions Qualification of staff Establish and maintain a quality control system Monitoring corrective measures Documentation 32

33 Slide 21 Questions? Slide 22 Specific measures Plastics 33

34 Slide 23 Plastics First material type to be covered by specific measures Directive 82/711/EEC basic rules for testing migration Directive 85/572/EEC list of simulants to be used for testing migration Directive 90/128/EEC Directive 2002/72/EC Regulation (EU) No. 10/2011 Slide 24 Regulation (EU) No 10/2011 scope Plastics Plastic multi-layer materials Printed and coated plastics Plastic layers or coatings forming a gasket in a cap or closure Plastic layers in multi-material multi-layer materials Printing inks Adhesives NOT Ion exchange resins Coatings Rubber Silicones 34

35 Slide 25 Reg. (EC) No 10/2011 principle of safety Specific authorisation of substances Suitable technical quality and purity of substance Restrictions Specific migration limit (SML) Maximum permitted quantity in the material (QM) Overall migration limit (OML) Other restrictions and specifications Substances in nanoform shall only be used if explicitly authorised Slide 26 Reg. (EC) No 10/2011 principle of safety List of substances authorised for use in plastic food contact materials and articles shall contain: Monomers and other starting materials Macromolecules from microbial fermentation Additives NO Colorants Polymer production aids Solvents Those not in list Subject to national law Substances that may be present in plastic materials: Non-intentially added substances Aids to polymerisation 35

36 Slide 27 Reg. (EC) No 10/2011 principle of safety Substances not listed but authorised for use in plastic food contact materials and articles Salts of authorised acids, phenols, alcohols with Al, Ba, Ca, Co, Cu, Fe, K, Li, Mg, Na, Zn Mixtures of authorised substances without chemical reaction Pre-polymers and natural and synthetic macromolecules of authorised monomers or starting substances: for use as monomers or starting substances natural and synthetic polymeric substances with M r 1000 g/mol for use as additive Complying requirements regulation Function as main structural component of final material Slide 28 Reg. (EC) No 10/2011 Specific migration Specific migration = the amount of a substance released from a material into food Limit expressed in mg/kg No limit SML = 60 mg/kg Additives also authorised as food additives or flavourings In authorised foods: shall not exceed restrictions/sml in Reg. (EC) No 1333/2008, Reg. (EC) No 1334/2008 or this Reg. Annex I In non-authorised foods: shall not exceed restrictions/sml in this Reg. Annex I 36

37 Slide 29 Reg. (EC) No 10/2011 Principle of inertness Overall migration = total amount of all non-volatile substances released from a material into food Limit: 10 mg/dm 2 Infants, young children (0-3) Limit: 60 mg/kg food Slide 30 Reg. (EC) No 10/2011 functional barrier Layers not in contact with food and separated from food by a functional barrier may be manufactured with substances not listed, but not: mutagenic, carcinogenic, toxic to reproduction in nanoform Specific migration not detectable with statistical certainty and a LoD of 0.01 mg/kg LoD shall also apply to a group of substances that are structurally and toxicologically related Limit includes set-off transfer 37

38 Slide 31 Migration test result Reg. (EC) No 10/2011 expression of results N Cap, gasket, etc.? N V < 0.5L or Y >10L or S/V inestimable Intended mg/kg * Y use known? actual Y content For children? N For Y children? mg/kg Y mg/kg actual content S/V =6 *** *** * DRF may be applicable provided SML N.D. FRF may be applicable provided SML N.D and not intended for children (<3 years) and food fat content >20% N OM? Y Cap, gasket, etc? Y For Y N N children? Intended use known? N mg/kg mg/article Y mg/dm 2 actual content ** mg/dm 2 total N surface article ** + cap mg/kg actual content or mg/dm 2 total surface article + cap * ** *** DRF may be applicable provided SML N.D N ** DRF may be applicable Slide 32 Reg. (EC) No 10/2011 new Revised list of food simulants non-acidic, non-alcoholic, non-fatty foods simulant is 10% ethanol alcoholic foods containing up to 20% alcohol simulant is 20% ethanol dairy, cloudy, and high-alcohol beverages simulant is 50% ethanol fatty foods simulant is vegetable oil (meeting certain specifications) acidic food simulant is 3% acetic acid dry foods simulant is poly(2,6-diphenyl-p-phenylene oxide), commonly known as Tenax TA 38

39 Slide 33 Reg. (EC) No 10/2011 new Migration test conditions for storage >30 10 in Directive 2002/72/EC has been revised: 10 for storage 6 10 for storage 6 Depending phase transition temperature of polymer 10 scientific evidence that migration has reached equilibrium under this test condition Separate test conditions for verifying compliance with OML and SML OML: fewer combinations of contact time and temperature Slide 34 Implementation of technical changes Until 31 December 2012, compliance documents should be based on migration testing using: food simulants specified in 85/572/EEC and test conditions specified in 82/711/EEC From 1 January December 2015, compliance documents should be based on migration testing using: food simulants specified in the (EC) No. 10/2011 and test conditions specified in 82/711/EEC or test conditions established in the (EC) No. 10/2011 From 1 January 2016, compliance documents should be based on migration testing using: food simulants + test conditions specified in (EC) No. 10/

40 Slide 35 Reg. (EC) No 10/2011 amendments Regulation (EU) No 321/2011 bans the use of Bisphenol A (BPA) for the manufacture of polycarbonate infant feeding bottles Regulation (EU) No 1282/2011 Melamine SML: mg/kg And others Slide 36 Regulation (EU) No 284/2011 Applicable to polyamide and melamine plastic kitchenware that falls under CN code ex Primary aromatic amine release from polyamide kitchenware Formaldehyde release from melamine-ware Products originating in or consigned from China and Hong Kong are controlled Prior Notification by importer is required to notify competent authority of the estimated date and time of physical arrival of the consignment 2 working days in advance Documentary checks on 100% of consignments Identity and physical checks on 10% of consignments Random selection including laboratory testing 40

41 Slide 37 Regulation (EC) No 1835/2005 Epoxy derivatives (BADGE, BFDGE, NOGE) Scope Plastics NOT Coatings Containers or storage tanks >10 m Adhesives 2 Use and presence of BFDGE, NOGE prohibited BADGE, BAGDG H 2 O, BAGDG 2H 2 O SML = 9 mg/kg or 9 mg/6 dm 2 (V<500ml v V>10 l) BADGE HCl, BAGDG 2HCl BAGDG H 2 O HCl SML = 1 mg/kg or 1 mg/6 dm 2 (V<500ml v V>10 l) Appropriate labelling with date of filling Slide 38 Questions? 41

42 Slide 39 Specific measures regenerated cellulose Slide 40 Regenerated cellulose films Directive 2007/42/EC Positive lists Restrictions on the substances but not OML Declaration of compliance 42

43 Slide 41 Specific measures ceramics Slide 42 Directive 84/500/EEC Ceramics Rules for migration testing (4% acetic acid) and analysis Migration limits for lead and cadmium Compliant if one exeeds >50% of limit, but average of 3 others are below limit and not exceedding >50% of limit DoC Type Type of article Lead Cadmium Type 1 Articles not fillable or 0.8 mg/dm² 0.07 mg/dm² H< 25 mm Type 2 Articles fillable H>25 mm 4.0 mg/l 0.3 mg/l Type 3 Cooking Ware Packaging/Vessels V>3L 1.5 mg/l 0.1 mg/l 43

44 Slide 43 Specific measures substances Slide 44 Directive 93/11/EEC N-nitrosamines and N-nitrosatable substances in elastomers and rubber teats and soothers Rules for migration testing and analysis SML = 0.01 mg released N-nitrosamines /kg material SML = 0.1 mg released N-nitrosatable substances /kg material 44

45 Slide 45 Recycled plastics Slide 46 Recycled plastics Requirements Scope: Mechanical recycling Individual authorization of recycling process Quality of input Efficiency of the process of decontamination (challenge test) Restriction on the recyclate Evaluation by EFSA of the recycling process Requirements of the quality assurance system Voluntary labelling Declaration of compliance for the recyclate and for the finished article 45

46 Slide 47 National Laws Slide 48 National rules may derive: National laws for all the EU Member States from harmonized EU rules for some EU Member States from pre-existing national laws or for new laws in sectors not yet harmonized The DG SANCO website gives information on the national laws of the Member States 46

47 Slide 49 National laws Member States FRANCE BELGIUM GERMANY ITALY SPAIN NETHERLANDS Several décrets,... Arrêtés royaux 11/5/92 & 3/7/2005 BFR Decreto 21/3/1973 +Amendments RESOLUCION 4/11/1982 warenwet Plastics Cleaning agents Coatings Elastomers& rubbers Ionisation Metals Paper& Paperboard RCF Wood Plastics Tin RCF Paper & Paperboard Ceramics Glass Lebensm. und Futterm. BGBI + 53 BFR Recommend. (By Polymer Type) + Paper & Paperboard rec xxxvi Plastics Rubbers RCF Macromolec. Paper& Compounds Paperboard Glass Stainless steel Plastics Ceramics Coatings Elastomers Glass Metal Paper&Board RCF Textile Wood Slide 50 Other EC bodies and European organisations involved in FCM control 47

48 Slide 51 JRC and EU Reference Laboratory Risk management (SANCO) As FCM activities 16 years Serving sectorial policies on release of substances from food contact materials Work Methods, migration data, scientific support for FCM legislation Ad-hoc contributions to EFSA for exposure assessment Official controls Member State Authorities and Enforcement Laboratories As EU Reference Laboratory Work Supporting Regulation 882/2004 on official food controls Member State authorities and enforcement Laboratories (NRLs) Slide 52 FVO Food and Veterinary Office (FVO) checks on compliance with the requirements of EU food safety and quality, animal health and welfare and plant health legislation within the European Union and on compliance with EU import requirements in third countries exporting to the EU contributes to the development of European Community policy in the food safety, animal health and welfare and plant health sectors 48

49 Slide 53 FVO Food and Veterinary Office (FVO) contributes to the development and implementation of effective control systems in the food safety, animal health and welfare and plant health sectors informs stakeholders of the outcome of its audits and inspections Each year the FVO develops an inspection programme, identifying priority areas and countries for inspection Slide 54 Council of Europe CoE is an European institution and is not the EU/EC 48 countries adhere to the CoE These documents are not legally binding unless they are transposed into national laws However the majority of Member States recognise their validity in absence of EU and/or national rules 49

50 Slide 55 Inventory Resolution AP(89)1: colorants in plastics Resolution AP(92)2: aids to polymerization for plastics Resolution AP(2002)1: paper and board Guidelines: metals and alloys Resolution AP(2004)1: coatings Resolution AP(2004)2: cork Resolution AP(2004)3: ion exchange resins Slide 56 Inventory Resolution AP(2004)4: rubber Resolution AP(2004)5: silicones Resolution AP(2005)2: packaging inks Guidelines: glass Guidelines: paper kitchen towels and napkins 50

51 Slide 57 Council of Europe The majority of the materials regulated by CoE are composed of: Inventory Lists (less or more complete) Rules for migration testing Industrial GMP Practical Guide Slide 58 Inventory lists Composed of: Substances authorised initially by EU countries, evaluated by EFSA and authorized by EU measures (List 1) Substances approved by EU countries but not yet by EFSA and EU (appendix to List 1) Other substances requested by industry but not yet accompanied by the necessary documentation (List 2) 51

52 Slide 59 Council of Europe Rules for migration testing are inserted in a Technical Document which is approved only by the Committee and, then, easily amendable. These rules are often those of the EU for plastics but derogation are permitted, if technically justified "Practical Guide" is also a Technical Document the aim of which is to explain the Resolution and to give further detailed recommendations in its application Slide 60 Council of Europe "GMP documents are prepared by industry but examined also by the Committee which inform all the stakeholders on how the product under consideration is manufactured 52

53 Slide 61 Council of Europe Resolutions Example paper and board Slide 62 Paper and board Res. AP (2002)1: General requirements Tech Doc No 1: Tech Doc No 2: Tech Doc No 3: Tech Doc No 4: Tech Doc No 5: List of substances (incomplete) Guidelines on test conditions and methods of analysis Guidelines for recycled fibres The CEPI Guide for GMP Practical Guide 53

54 Slide 63 Paper and board Inventory lists SML and other restrictions are applicable No OML GMP Suitable microbiological quality No release of substances having an antimicrobial effect Slide 64 Paper and board Recycled fibres can be used (a) if it originates from specified qualities; (b) if they are subject to appropriate processing and cleaning (c) finished materials comply with the restrictions in the Resolution 54

55 Slide 65 CEN CEN standard methodology Overall migration test methods Analytical methods (standards and technical specification) for testing compliance with SML and QM restrictions Slide 66 RASFF Rapid Alert System for Food and Feed (RASFF) Was 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 55

56 Slide 67 Useful links Website on legislation (SANCO) /index_en.htm Website on migration testing (JRC) Website on risk assessments (EFSA) Council of Europe Slide 68 New tool: Commission Database 56

57 Slide 69 The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States 57

58 Lecture 3: Procedure and testing requirements for importing FCM in the EU. Slide 1 Procedure and testing requirements for importing FCM in the EU Catherine Simoneau Slide 2 Overview Regulatory requirements, particular related to testing, for importers who wish to import FCM into EU Procedure for importers who intend to import FCM into EU Requirements of testing laboratories for performing compliance testing to EU legislative requirements Implementation timelines and details of the legislative requirements Sampling plans for a shipping lot 58

59 Slide 3 Overview Regulatory requirements, particular related to testing, for importers who wish to import FCM into EU All EU legislation described in the previous presentation is applicable Procedure for importers who intend to import FCM into EU Declaration of compliance Analytical test reports demonstrating compliance Slide 4 How to export a product into Europe Product (material type) fully regulated at EU level Demonstrate compliance with the EU legislation previously described Product (material type) fully regulated at National level in one Member State Demonstrate compliance with the national legislation provided Product (material type) fully regulated at National level in more than one Member State Demonstrate compliance with the national legislation of the country that has the most severe rules and apply the principle of mutual recognition 59

60 Slide 5 Principle of mutual recognition Any product lawfully produced and marketed in one Member State must be admitted to the market of any other Member State Member State can block under certain conditions the importation of products for protection of public health environmental and other reasons Slide 6 How to export a product into Europe Product (material type) not regulated at EU or National level accompany the product with adequate documentation showing that the product is safe References documents such as FDA approval, other national recognised legislation and Council of Europe Resolutions, described later 60

61 Slide 7 Testing requirements Requirements of the Framework Regulation Requirements of the GMP Regulation Is the material type specifically regulated at EU level? If so which legislation is applicable? Slide 8 Testing requirements Have any restrictions been placed on the starting substances used to make the material or article? Which tests should be carried out? 61

62 Slide 9 Requirements of the Framework Regulation Labelling Traceability Declaration of compliance Good manufacturing practice Slide 10 Requirements of the GMP Regulation GMP means those aspects of quality assurance which ensure that materials and articles are consistently produced and controlled to ensure conformity with the rules applicable to them and with the quality standards appropriate to their intended use by not endangering human health or causing an unacceptable change in the composition of the food or causing a deterioration in the organoleptic characteristics thereof 62

63 Slide 11 Example nylon kitchen utensils Is the material type regulated at EU level by a specific measure? Yes, nylon is a plastic If so which legislation is applicable? Framework Regulation (EC) No 1935/2004 Plastics Regulation EU No 10/2011 Regulation (EU) No 284/2011 Slide 12 Implementation of technical changes Transitional provisions for compliance testing From January 1, 2013 to December 31, 2015, compliance documents should be based on migration testing using: the food simulants established in the Regulation (EC) No. 10/2011 and the test conditions specified in 82/711/EEC, as amended, OR the test conditions established in the 10/2011 From January 1, 2016, compliance documents should be based on migration testing using: the food simulants and test conditions established in Regulation (EC) No. 10/

64 Slide 13 Requirements of testing laboratories Validated analytical methods Trained personnel Participation in proficiency test schemes where available Quality assurance Accreditation (e.g. ISO 17025) Slide 14 The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States 64

65 Lecture 4: Active and intelligent packaging Slide 1 Active and intelligent packaging Eddo J. Hoekstra Joint Research Centre The European Commission s in-house science service Slide 2 food contact materials Extend shelf-life of packaged food Maintain/improve condition of packaged food smart materials active materials Release or absorb substances into or from the packaged food or the environment surrounding the food intelligent materials Monitor the condition of packaged food or the environment surrounding the food 65

66 Slide 3 Benefits of smart materials Traditional packaging Passive barrier against microorganisms and chemicals Smart Packaging Reactive barrier against microorganisms and chemicals Maintain/improve condition of packaged food Colour Organoleptic properties Nutritional composition Ripening Deterioration Monitor the condition of packaged food or the environment surrounding the food Freshness Time-temperature Slide 4 Waste and recycling Longer shelf-life Less food waste? Recycling? Multi-material Multi-layer plastic 66

67 Slide 5 Regulation Active and Intelligent materials Slide 6 Active materials absorbers Carbon dioxide Microbial growth Ethene Ripening packaging Oxygen Microbial growth Water Deterioration of food Respiring food + fish/meat Environment Passive layer Active layer Food environment Food 67

68 Slide 7 Active materials releasers Carbon dioxide Ethanol anti-microbial Silver Sulphur dioxide packaging grapes Anti-oxidants Flavours Tin simulate canned tomatoes Nitrogen foam on beer Environment Passive layer Active layer Food environment Food Slide 8 Smart but not active materials Scavengers: Oxygen PET Acetaldehyde UV Releasers: Heat Beverages + microwave food Material active or not? Depends on claim of producer Material should protect the food Not material Not against environment Environment Active layer Passive layer Food environment Food 68

69 Slide 9 Placing on the market Suitable and effective for the intended purpose of use Good Manufacturing Practice no transfer of their constituents into food in quantities which could: endanger human health bring about an unacceptable change in the composition of the food bring about a deterioration in the organoleptic characteristics thereof Labelling, advertising and presentation of a material or article shall not mislead the consumers. Slide 10 Placing on the market Allowance of changes in the composition or organoleptic characteristics of food on condition that the changes comply with the Community (or national) provisions applicable to food No misleading masking the spoilage of food (active) condition of the food (intelligent) Adequately labelling to allow identification of non-edible parts DO NOT EAT (min font 3 mm) + label materials or articles are active/intelligent 69

70 Slide 11 Risk management of substances Authorisation by relevant Community provisions applicable to food Substances not actively released, grafted or behind FB Released active substances intended to be released Substances falling within the scope of Community or national provisions applicable to food, which are grafted or immobilised in order to have a technological effect in the food EU list Authorisation procedure Substances used in components which are not in direct contact with food and are separated from the food by a functional barrier Substances classified as mutagenic, carcinogenic, or toxic to reproduction Regulation (EC) No 1272/2008 Substances deliberately engineered to nano-particle size Discuss here the examples of the guideline on AIM Slide 12 EU List substances Submission of applications for the safety assessment of substances to the European Food Safety Authority Public registry available with all substances having a valid application EFSA will deliver its opinion on all substances included in the register The Commission will establish the community list Identity of the substance(s) Function of the substance(s) Reference number If necessary: Conditions of use of the substance(s) or component Restrictions and/or specifications of use of the substance(s) Conditions of use of the material to which the substance or component is added or into which it is incorporated Slide 13 70

71 Non-Community List substances Conditions of use of substances: intended to be released into food Grafted/immobilised on the active material with the intention of a technological effect on food Full compliance with relevant Community and national provisions applicable to food and provisions in Regulation (EC) No 1935/2004 Amount of release shall not be included in measured overall migration If substance is listed in e.g. plastic food contact material list, the amount released may exceed this specific restriction provided compliance with Community or national provisions for foods Slide 14 Non-Community List substances Conditions of use of substances: in indirect contact (behind functional barrier) Migration shall not exceed 0.01 mg/kg food This limit applies to a group of substances if they are structurally and toxicologically related Not classified as mutagenic, carcinogenic or toxic to reproduction (EC No 1272/2008) Not nanoparticles 71

72 Slide 15 Compliance Compliance of substance in component AIM Check substance is approved under Additive Regulation 1333/2008 Flavour Regulation 1334/2008 Y Y Enzyme Regulation 1332/2008 Released? N Technol. effect on food? N Y No active component Grafted or immobilised? N compliance? Y Compl. prov. national leg.? Y N N Substance released? Y N Y CMR or nano? N N Specific migration 0.01 mg/kg? Behind functional barrier? Y N Compl. prov. 1935/2004? Y N Not compliant Compliant Y N Compliance restrictions in EU list 450/2009? Y Slide 16 Risk management of anti-microbials To be clarified yet Applicable 1/9/2013 Anti-microbials in food contact materials Application 5-chloro-2-methyl-2Hisothiazol-3-one, mixture with 2-methyl-2Hisothiazol- 3-one (3:1) in coating, paper Surface anti-microbial Authorisation under 528/2012 Ag zeolitea in PO, PET, PC Process anti-microbial Polymer production aid Food preservative Active material Max residue limit in food Plastic FCM Authorisation under national law Reg. 450/2009 Non-mandatory authorisation under 10/2011 Authorisation under 1333/2008 Use 72

73 Slide 17 Declaration of compliance All materials/components/substances Issued by the business operator at every marketing stage in the production chain except when sold to consumers Appropriate documentation demonstrating compliance Suitability Effectiveness Test conditions and results Calculations Other analysis an evidence on safety Reasoning Slide 18 EFSA opinions on active substances Register of substances with a valid application for authorisation Moisture and liquid absorbers Open-cell expanded polystyrene, talc, alkyl(c 8 -C 22 )sulphonic acid salts for fresh fish, meat, poultry (EFSA J ) Na carboxymethylcellulose, bentonite, KAl(SO 4 ) 2 12H 2 O for not direct food contact (EFSA J ) 73

74 Slide 19 EFSA opinions on active substances Oxygen scavengers Na borohydride, Pd acetate in plastic (EFSA J ) activated carbon, H 2 O, Fe powder, kaolin calcined, sulphur NaCl in sachet (EFSA J ) (terephthalic acid, dimethyl ester, polymer with 1,4- butanediol, cyclized, polymers with glycidyl methacrylate, hydroxyl-terminated polybutadiene, methyl methacrylate and styrene) copolymer and cobalt stearate (catalyst) in PET (EFSA J ) Fe(II) modified bentonite in plastic or sachet (EFSA J ) Slide 20 Entry into force and application 19 June 2009 Entry into force From 19 December 2009 Declaration of Compliance according to Regulation Non-edible parts labelled according to Regulation labelled according to EC No 1935/2004 before 19/12/2009 marketing until exhaustion of stocks Date of application of Community List ( 2011) < Authorise and use according to relevant Community provisions applicable to food and EC No 1935/2004 > Composition requirements apply 74

75 Slide 21 Questions Thank you! Slide 22 The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States 75

76 Lecture 5: Testing compliance: migration testing for plastics Slide 1 Testing compliance: migration testing for plastics Catherine Simoneau Slide 2 Overview Food simulants and correspondence foods simulants Time temperature conditions Guidelines for interpretation of test conditions Testing type Overall migration testing Testing for fatty contact 76

77 Slide 3 Testing strategies Analysis of the material or article Analysis of foods Analysis of food simulants The packaging can be tested for its suitability before use by employing food simulants that are intended to mimic the migration properties of different categories of foods Introduced in the early-1980 s along with the rules for using simulants Slide 4 screening tests Alternative extraction tests indicated are permissible instead of migration tests with fatty food simulant when the results obtained in a comparison test' show that the values are equal to or greater than those obtained in the test with simulant D Any solvent/test conditions as long as the alternative extraction test result is higher 77

78 Slide 5 Food simulants Food simulant" means a test medium imitating food; in its behaviour the food simulant mimics migration from food contact materials Designed to overestimate the migration into foods Slide 6 Which simulant? Regulation (EU) No 10/2011 Aqueous foods = Simulant A 10% (v/v) aqueous ethanol Acidic foods (< ph 4.5) = Simulant B 3% (w/v) aqueous acetic acid Alcoholic foods (< 20% alcohol) = Simulant C 20% (v/v) aqueous ethanol Foods with an alcohol content of above 20% and for oil in water emulsions = Simulant D1 50% (v/v) aqueous ethanol Simulant D2 vegetable oil Dry foods= Tenax 78

79 Slide 7 Slide 8 Assignment of simulants vs foods 79

80 Slide 9 Overall migration Overall migration limit of 60 mg/kg Because a test for overall migration using food simulants is entirely conventional i.e. the test result depends on the method used the standard test procedures have to be used and followed exactly CEN standards Slide 10 Reg. (EU) No 10/2011: simplified scheme for OM Test Contact time in days [d] or hours [h] at Contact temperature in [ºC] Intended food contact conditions OM 1 10 d at 20 C Any food contact at frozen and refrigerated conditions. OM2 10 d at 40 C Any long term storage at ambient temperature or below, including heating up to 70 C for up to 2 hours, or heating up to 100 C for up to 15 minutes. OM3 2 h at 70 C Any contact conditions that include heating up to 70 C for up to 2 hours, or up to 100 C for up to 15 minutes, which are not followed by long term room or refrigerated temperature storage. OM4 1 h at 100 C High temperature applications for all food simulants at temperature up to 100 C. OM5 2 h at 100 C or at reflux or alternatively 1 h at 121 C High temperature applications up to 121 C. OM6 4 h at 100 C or at reflux Any food contact conditions with food simulants A, B or C, at temperature exceeding 40 C. OM7 2 h at 175 C High temperature applications with fatty foods exceeding the conditions of OM5. 80

81 Slide 11 Navigating options: OM Overall migration Screening approach Migration testing Choose simulants(s) Solvent extraction # A, B, C, D1 D2 Select exposure Select exposure conditions * conditions * Calculate total mass of extractable substances Perform migration test Perform migration test Mass < OML? Yes No Material compliant Migration < OML? Migration test technically feasible? Yes No Yes No Material Material compliant not compliant Migration < OML? Yes No Perform tests with substitute simulants * Exposure conditions may be conventional conditions or accelerated test conditions using defined acceleration factors # The results of solvent extraction tests may be used to demonstrate compliance with the legislative limit, provided that the result obtained in a comparison test shows that the value is equal to or greater than those obtained in the migration test with a conventional food simulant; Material Material compliant not compliant Migration < OML? Yes No Material Material compliant not compliant Slide 12 OM special cases of simulant assignment 81

82 Slide 13 Specific migration Positive list of monomers, other starting substances and additives permitted for use in the manufacture of plastic for food contact This list contains any limits on the migration of individual or groups of substances limits that have been assigned following the toxicological assessment of these substances Slide 14 Compliance with specific migration limits Determination of the concentration of the substance(s) in the polymer Calculation of total transfer Migration modelling Determine the migration into food simulants Determine the migration into foods 82

83 Slide 15 Concentration in the polymer QM and QMA restrictions e.g. Isocyanates Volatiles Reacts with food or food simulant Demonstrate complete extraction Polymer dissolution and subsequent precipitation Successive solvent extraction Selection of extraction solvent dependent on both the polymer and the substance cp,0 Slide 16 Migration modelling Based on diffusion theory and a consideration of partitioning effects Diffusion coefficient of the migrant in the plastic (DP) Partition coefficient of the migrant between the plastic and the food or food simulant (KP,F) 83

84 Slide 17 Navigating options: SM Specific migration materials not in contact with foods Screening approach Migration testing Solvent extraction # Parameters known for migration modelling? Choose simulants(s) A, B, C, D1 D2 Determine cp,0 and QM Yes No Select exposure Select exposure conditions * conditions * Perform modelling Calculate migration assuming 100% transfer Migration < SML? Perform migration test erform P migration test Migration < SML? Yes No Material compliant Yes Material compliant No Migration < SML? Yes No Migration test technically feasible? Yes Material Material compliant not compliant Migration < SML? No Not in core text of R10/2011 Perform testswith substitute simulants Yes No * Exposure conditions may be conventional conditions or acceler ated test conditions using defined acceleration factors # The results of solvent extraction tests may be used to demonstrate compliance with the legislative limit, provided that the result obtained in a compar ison test shows that the value is equal to or greater than those obtained in the migratio n test with a conventional food simulant; Material Material compliant not compliant Migration < SML? Yes No Material Material compliant not compliant Slide 18 Test conditions: time of exposure 84

85 Slide 19 Test conditions: temperature of exposure Slide 20 Long term storage 10 days at 20 C: Frozen foods 10 days at 40 C: 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 10 days at 50 C: storage time at cooled 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 85

86 Slide 21 Specific cases Contact conditions generally recognized as more severe Contact with foodstuffs at any condition of time and temperature Contact with foodstuffs at room temperature or below for an unspecified period Contact in a microwave oven Slide 22 Specific cases Contact conditions causing changes in physical or other properties Contact for less than 15 min at temperatures between 70 C and 100 C 86

87 Slide 23 Now in practice: OM and SM Slide 24 Migration testing Pouch testing Total immersion test Single face immersion cell Article filling Support for strips 1 dm2 cutting template 87

88 clamp bar base plate clamp screw filler plug food simulant rubber mat lid sealing ring ¼C Slide 25 Migration testing simulant Double face testing by immersion 1 dm 2 S1 S2 S3 B1 B2 Single surface testing using cells cell at Tº + liquid at T Single surface testing using pouches 10 x 10 cm hole + simulant at Tº + + wire gauze support 120 seal pouch: sides in contact with simulant facing pouch holder at Tº S1 S2 S3 B1 B2 Type A (Pira cell) Type B (TNO cell) article filling equilibrated at Tº EXPOSURE (t, T) Slide 26 Testing set-ups for time temperature exposures Single cell and simulant Total immersion in olive oil Foods in glass single face cell (e.g. rigid films) 88

89 Slide 27 Sampling and testing Slide 28 Sampling overall migration Overall migration Four test specimens for the test for each simulant Two additional test specimens to determine loss of volatiles when testing using simulant D One additional test specimen to determine the suitability of olive oil as the fatty food simulant and triheptadecanoin as the internal standard If the articles are an irregular shape then another two test specimens are required to determine the surface area 89

90 Slide 29 Sampling specific migration Specific migration Not well defined Recommendations in the EURL-NRL guidelines are based on Directive 2004/16/EC laying down the sampling methods and the methods of analysis for the official control of the levels of tin in canned foods Slide 30 Selection of test conditions Compliance testing is SIMULATION of WORST case migration into food Appropriate selection of test conditions is VERY important to obtain COMPARABLE test results and correct evaluation food contact materials 90

91 Slide 31 Standard methods Slide 32 Recognised methods Community methods = methods laid down in the legislation (only for ceramics) Internationally recognized: CEN Reliable, collaboratively tested, to be used in case of dispute EN 1186 Overall migration plastics EN Specific migration plastics TS polymeric coatings and others Link CEN: Other technical specifications Directives (ceramics, vinyl chloride) CoE guidelines, national legislations or recommendations 91

92 Slide 33 CEN methods overall migration Standard reference Title Plastics Materials and articles in contact with foodstuffs - Plastics - EN :2002 Part 1: Guide to the selection of conditions and test methods for overall migration EN :2002 EN :2002 EN :2002 EN :2002 EN :2002 EN :2002 EN :2002 EN :2002 EN :2002 EN :2002 EN :2002 EN :2002 EN :2002 EN :2002 Part 2: Test methods for overall migration into olive oil by total immersion Part 3: Test methods for overall migration into aqueous food simulants by total immersion Part 4: Test methods for overall migration into olive oil by cell Part 5: Test methods for overall migration into aqueous food simulants by cell Part 6: Test methods for overall migration into olive oil using a pouch Part 7: Test methods for overall migration into aqueous food simulants using a pouch Part 8: Test methods for overall migration into olive oil by article filling Part 9: Test methods for overall migration into aqueous food simulants by article filling Part 10: Test methods for overall migration into olive oil (modified method for use in cases where incomplete extraction of olive oil occurs) Part 11: Test methods for overall migration into mixtures of C-labelled synthetic triglycerides Part 12: Test methods for overall migration at low temperatures Part 13: Test methods for overall migration at high temperatures Part 14: Test methods for 'substitute tests' for overall migration from plastics intended to come into contact with fatty foodstuffs using test media iso-octane and 95 % ethanol Part 15: Alternative test methods to migration into fatty food simulants by rapid extraction into iso-octane and/or 95 % ethanol Slide 34 CEN methods Overall migration aqueous 1. Glassware weight empty (m1) S1 S2 S3 B1 B2 mbs1 mbs2 mbs3 mbb1 mbb2 2. Sample preparation x 7 samples 3. Exposure to food simulant (t, T) 4. Removal of specimens, take residual liquid S1 S2 S3 B1B2 L1 S1 S2 S3 B1 B2 5. Slow evaporation of liquid (hot plate) S1 S2 S3 B1 B2 Exposure to test simulant, evaporation to dryness, weight of residue Overall migration: determined by the mass of residue after evaporation of the food simlant M = (m a -m b ) x 1000 mg/dm 2 S S1 S2 S3 B1 B2 L0 simulant 6. oven-dessicator to weight final mass (m2) S1 S2 S3 B1 B2 mbs1 mbs2 mbs3 mbb1 mbb2 Valid and reproducible results require expertise 92

93 Slide 35 CEN methods Overall migration oil 1. Sample weight before exposure (m1) S1 S2 S3 S4 B1 B2 E1 E2 simulant 4. Extraction of absorbed oil (soxhlet) 5. Derivatisation of absorbed oil by fatty acid methyl esters (FAME) x 7 samples record repeat FAME masse with 6 s: m a standards 0-50 mg oil (C17 spiked) for H20 H20 calibration 2. Exposure to food H20 curve simulant (t, T) H20 6. GC-FID determination of absorbed oil by FAME -> m3 empty tubes: adjust for loss of volatiles 3. Remove free oil & weight sample (m2) E L Bradley, Hong Kong Seminar May Overall migration: Determined by weight loss of specimen M = (m a -(m b -m c )) x 1000 mg/dm 2 S Valid and reproducible results require expertise Slide 36 Check points Overall migration in oil Stable weight of test sample (conditioning of sample) Test temperature according of the analytical tolerances Extraction efficiency of the oil Linearity of calibration curve C18/C16 ratio of extracted oil check for interferences Individual results must be within analytical tolerance 93

94 Slide 37 Specific migration Determination of quantity after migration of a specific substance (targeted analyses) 3 steps: extraction, clean-up (if necessary), determination Analytical approach depends on: Volatility and polarity of the substance Nature of food simulant Level of determination Functional groups of the substance Slide 38 Specific migration Lowest sensitivity (non-detectable): 10 µg subst / kg food Source of analytical methods: CEN (series EN for plastics) EU Reference Laboratory web site: 94

95 Slide 39 SM: plastics (1) Standard reference Title Plastics Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - EN :2004 Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food simulants and the determination of substances in plastics and the selection of conditions of exposure to food simulants EN :2004 Part 2: Determination of terephthalic acid in food simulants EN :2004 Part 3: Determination of acrylonitrile in food and food simulants EN :2004 Part 4: Determination of 1,3-butadiene in plastics EN :2004 Part 5: Determination of vinylidene chloride in food simulants EN :2004 Part 6: Determination of vinylidene chloride in plastics EN :2004 Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants EN :2004 Part 8: Determination of isocyanates in plastics CEN/TS :2005 Part 9: Determination of acetic acid, vinyl ester in food simulants CEN/TS :2005 Part 10: Determination of acrylamide in food simulants Slide 40 SM: plastics (1) Standard reference Title Plastics Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - CEN/TS :2005 Part 11: Determination of 11-aminoundecanoic acid in food simulants CEN/TS :2005 Part 12: Determination of 1,3-benzenedimethanamine in food simulants CEN/TS :2005 Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants CEN/TS :2005 Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulants CEN/TS :2005 Part 15: Determination of 1,3-butadiene in food simulants CEN/TS :2005 Part 16: Determination of caprolactam and caprolactam salt in food simulants CEN/TS :2005 Part 17: Determination of carbonyl chloride in plastics CEN/TS :2005 Part 18: Determination of 1,2-dihydroxybenzene, 1,3-dihydroxybenzene, 1,4-dihydroxybenzene, 4,4'- dihydroxybenzophenone and 4,4'dihydroxybiphenyl in food simulants CEN/TS :2005 Part 19: Determination of dimethylaminoethanol in food simulants 95

96 Slide 41 SM: plastics (2), paper and board Standard reference Title Plastics Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - CEN/TS :2005 Part 20: Determination of epichlorohydrin in plastics CEN/TS :2005 Part 21: Determination of ethylenediamine and hexamethylenediamine in food simulants CEN/TS :2005 Part 22: Determination of ethylene oxide and propylene oxide in plastics CEN/TS :2005 Part 23: Determination of formaldehyde and hexamethylenetetramine in food simulants CEN/TS :2005 Part 24: Determination of maleic acid and maleic anhydride in food simulants CEN/TS :2005 Part 25: Determination of 4-methyl-1-pentene in food simulants CEN/TS :2005 Part 26: Determination of 1-octene and tetrahydrofuran in food simulants CEN/TS :2005 Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulants CEN/TS :2005 Part 28: Determination of 1,1,1-trimethylolpropane in food simulants Slide 42 Detection of migratable substances Range of substances with migration limits assigned means in turn that a range of analytical methods are deployed in testing; Headspace GC-MS for the volatiles GC-MS for the semi-volatiles LC-MS for the non-volatiles and the polar residues The detection level needed depends on the toxicological or organoleptic properties 96

97 Slide 43 Other considerations Simulant D (and its substitutes) reduction factor numbers, 2 to 5, which may be applied to the result of the migration tests relevant to certain types of fatty foodstuffs and which is conventionally used to take account of the greater extractive capacity of the simulant for such foodstuffs Slide 44 Other considerations Fat reduction Factor (FRF) The exposure to substances migrating predominantly into fatty food (lipophilic substances) was previously based on the general assumption that a person ingests daily 1 kg of food. However, a person ingests at most 200 g of fat on a daily basis FRF applicable to lipophilic substances Applicable substances listed in Directive 2002/72/EC, as amended 97

98 Slide 45 Testing for fatty contact For certain foodstuffs if it can be demonstrated that the foodstuff does not make fatty contact with the plastic then testing with simulant D is not required This is determined by placing food in contact with a polyethylene film containing a fat-soluble fluorescent dye. The degree of transfer of the dye from the film is related to the extent of fatty contact made, and is used to determine whether simulant D be employed or not CEN standard methodology Slide 46 Summary Numerous approaches to demonstrate compliance Dependent on the type of limit defined in the legislation Testing the material itself (worst case calculation and migration modelling), testing the foodstuff, exposing to and testing food simulants Worst foreseeable conditions of use Careful consideration of the migration results 98

99 Slide 47 Example 1. Nylon kitchen utensils Nylon kitchen utensils have the potential to come into contact with all food types aqueous, alcoholic, acidic and fatty Most migration testing on these articles has previously been carried out using 3% (w/v) aqueous acetic acid Generally accepted that this is the most severe simulant Utensils may be used in contact with acidic sauces/marinades Slide 48 Example 1. Nylon kitchen utensils Test conditions for food contact kitchen utensils are not well defined in the legislation or in the CEN guide EN13130 Part 1 Legislation has been interpreted differently in the various Member States (RASFFs) Task force within the EURL- NRL network to prepare guidelines defining the exposure conditions for articles intended for contact with food, including utensils 99

100 Slide 49 Example 1. Nylon kitchen utensils The worst foreseeable conditions of use for kitchen utensils are exposure to foods at temperatures in excess of 150 C for longer than 5 minutes but less than 30 minutes Slide 50 Exposure temperature 100

101 Slide 51 Exposure time Slide 52 Example 1. Nylon kitchen utensils Selected exposure conditions = 2 hours at 100 C 101

102 Slide 53 Example 1. Nylon kitchen utensils Total immersion of the utensil (not the handle) to avoid cut edges giving unrealistically high migration Articles exposed by total immersion to three successive portions of 3% acetic acid for 2 hours at 100 C Slide 54 Example 1. Nylon kitchen utensils As kitchen utensils are intended for repeat use then each article should be exposed to three successive portions of food simulant Articles exposed by total immersion to three successive portions of 3% acetic acid for 2 hours at 100 C 102

103 Slide 55 Example 2. Melamineware Contact with all food types Simulants B, C and D Article fill 0.5 mm from the rim Conditions defined in legislation for hot fill 2 hours at 70oC Repeat use Three successive exposures Slide 56 The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States 103

104 Lecture 6: Migration modelling for compliance testing of plastic FCM Slide 1 Migration modelling for compliance testing of plastic food contact materials Eddo J. Hoekstra 2500 Comparison margarine and olive oil vs. modelling Irganox 1076 ug/dm Margarine Olive oil margarine model olive oil model Days Joint Research Centre The European Commission s in-house science service Slide 2 Regulation (EC) No 10/2012 Compliance test Verification method Screening method Overall migration Residual content Migration modelling Food simulant substitutes Overestimation of modelled specific migration (section of Annex I) no FCM not yet in contact Compliant? yes OK Art December

105 Slide 3 Migration Diffusion Convection Evaporation Reaction Partitioning c t Diffusion is a good simplification for most food contact materials 4 December Slide 4 Monolayer one dimensional Fick s second law of diffusion 2 cp cp = DP 2 t x polymer food (simulant) At equilibrium (t= ) cp, ρ P K P, F = c ρ F, F 4 December

106 106 Slide 5 Boundary conditions Constant thickness of polymer film Polymer film in contact with finite volume of food (similant) and contact area Migrant homogeneously distributed in polymer at t=0 Neglecting mass transfer resistance at food (simulant) side Migrant homogeneously distributed in food (simulant) at t>0 No interaction between polymer and food (simulant) no swelling of polymer Diffusion coefficient of migrant in polymer is constant in place and time No migrant in food (simulant) at t=0 The amount of migrant in polymer + food (simulant) is constant 4 December ,0,, P P F m m m = + Slide 6 Analytical solution Maximum concentration in polymer Mass transfer equation 4 December Σ + = = t d D q q d c A m P P n n n P P P t F ,0, exp 1 ) ( α α α α α α ρ = = =,,,,, 1 P F P F P F P F P F F P m m V V c c V V K ρ ρ α n q n q α = tan exp 1 ) ( = Σ + = t d D q q d A V SML MIC P P n n n P P F F α α α α α α ρ ρ

107 Slide 7 Disadvantages of analytical solution Only monolayer Only mean concentrations in polymer and food (simulant) No successive contact cycles possible Repeated use articles Alternative Numerical solutions e.g. finite element or finite differences algorithms Analytical solution serves as reference for validation 4 December Slide 8 Multi-layer one dimensional Fick s second law of diffusion 9 1 cp = D t c c 2 2 P,1 P,2 P, 1 + D 2 P, x x + D P, n 2 c x P, n 2 polymer food(simulant) At equilibrium (t= ) K K Pn, F Pn + 1, Pn c = C Pn, F, F cp ρ n+ 1, Pn + 1 = c ρ ρ Pn, Pn ρ Pn 4 December

108 Slide 9 Estimation of diffusion coefficient Different approaches Arrhenius EA DP = D0 exp RT Estimation (Piringer) * * DP = exp AP M A * P τ AP T = '* 2 /3 r Polymer specific constant 10454R M r (m s RT 2 ) Polymer specific temperature constant Reference activation energy 4 December Slide 10 Estimation of A P for each T R. Brandsch, December

109 Slide 11 Estimation of A p * R. Brandsch, December Slide 12 Applicability for polyolefins c P,0 < 1% K P,F = 1 for high solubility of migrant in food. K P,F = 1000 for low solubility of migrant in food. Polymer T ( C) M r (Da) A P '* τ (K) LDPE LLDPE <80 < HDPE < PP (homo) PP (random) <120 < PP (rubber) < December

110 Slide 13 Polymer specific constant High A P High D P More flexible polymer 4 December Slide 14 Substances eligible for migration modelling All organic, non-gaseous substances with a well-defined molecular mass, soluble in the polymeric matrix All organic substances known to deliberately bloom out from some polymeric materials, e.g. antistatic or antifogging agents incorporated in polyolefines, at levels where blooming does not occur All specific substances in a mixture, typically derived from natural sources like fats and oils, rosins, waxes, starch, proteins, cellulose, cotton, with a well defined molecular mass below 2000 Da 4 December

111 Slide 15 Substances not eligible for migration modelling All organic substances known to deliberately bloom out from some polymeric materials, e.g. antistatic or antifogging agents incorporated in polyolefines, at levels where blooming occurs All organic mixtures with undefined molecular mass, typically derived from natural sources like fats and oils, rosins, waxes, starch, proteins, cellulose, cotton All inorganic substances, metals, metal oxides, metal salts, etc. 4 December Slide 16 Crucial information needed for migration modelling Polymer identity Potential substances that can migrate e.g. additives, residual amounts of monomers Initial concentrations worst-case intended use type of food maximum temperature maximum packaging time Intended highest surface-to-volume ratio 4 December

112 Slide 17 References ( Simoneau C. (ed) (2010) Applicability of generally recognised diffusion models for the estimation of specific migration in support of EU Directive 2002/72/EC, Publication Office of the European Union, Luxembourg, JRC Scientific and Technical Report, EUR EN Hoekstra E.J., Brandsch R., Dequatre C., Mercea P., Milana M.-R., Schaefer A., Simoneau C., Störmer A., Trier X., Vitrac O. (2012) Estimation of specific migration by generally recognised diffusion models in support of Regulation (EC) No 10/2011. In preparation Hoekstra E.J., Brandsch R., Dequatre C., Mercea P., Milana M.-R., Simoneau C., Störmer A., Trier X., Vitrac O. (2012) Technical guidance document to determine diffusion parameters to be used for migration modelling from plastics into foods. In preparation Hoekstra E.J., Brandsch R., Dequatre C., Mercea P., Milana M.-R., Simoneau C., Störmer A., Trier X., Vitrac O. (2012) Technical guidance document to determine the upper-limit temperature independent polymer specific constant (A p *) and 4 December polymer 2012specific activation temperature constant (t) for mathematical modelling 17 of a plastic food contact materials. In preparation Slide 18 The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States 112

113 Lecture 7: Correction factors of experimentally determined specific migration Slide 1 Correction factors of the experimentally determined specific migration Eddo J. Hoekstra Joint Research Centre The European Commission s in-house science service Slide 2 3 correction factors for specific migration 1. correction for the difference of surface-to-volume ratio between the experiment and the real food contact (Art. 17) 2. correction for the simulant D2 Reduction Factor (DRF) for defined foods (Section 4.2 of Annex V) 3. correction for the Fat Reduction Factor (FRF) for lipophilic substances migrating into food with a fat content of more than 20% (Section 4.1 of Annex V) Fat consumption is maximum 200 g D2 greater extraction capacity compared to food 4 December

114 Slide 3 Formula Surface-to-volume ration difference DRF = 1-5 (see Table 2 Annex III) M S/V = M test S V S V real test (mg/kg) FRF c = concentration fat in food (g fat/kg food) c max = maximum fat intake per day = 200 g fat/kg food c % = percentage of fat in food (% fat) > 20% FRF = 1-5 c 5 FRF = = c% c 100 max TRF = DRF FRF 5 4 December Slide 4 Conditions SML = ND no FRF applied Changes compared to Directive 2002/72/EC Specific migration is only expressed in mg/kg Even for V < 500 ml or V > 10 l Application DRF also when >80% migrates into food simulant D2 4 December

115 Slide 5 Compliance of experimental specific migration (M test ) N (S/V) test = (S/V) real?(dm²/kg) Y M S/V = M test (S/V) real /(S/V) test (mg/kg) M S/V = M test Food simulant A, B, C, D1, E? Y N Listed yes in column 7 of Table 1 of Annex I? N 1 Y food with 20% fat? Y N Contact with food for infants/young children? N S/V is impractical to estimate Y Y N 5 2 Slide 6 1 N Test with food? Y Food simulant D2? N Y SML=ND? N Select DRF Y M DRF = M S/V V<0.5 Yl v V>10 l v films N Y Y Child food? N Y M DRF = M S/V /DRF V<0.5 l v V>10 l v films N M S/V SML 60 mg/kg Y M=M S/V *6/(S/V) real Child food? Y N N M=M DRF *6/(S/V) real M DRF SML Y N N M SML 60 mg/kg Y M SML N Y Non-compliant Compliant 6 115

116 Slide 7 2 N Test with food? Y TRF=5 Y Select DRF Calculate FRF= g fat/kg food /200= % fat *5/100 TRF=FRF*DRF TRF>5 N M TRF =M S/V /TRF N M S/V 60 mg/kg Calculate FRF= g fat/kg food /200= % fat *5/100 Y N M FRF =M S/V /FRF V<0.5 l v V>10 l v films Y M=M S/V *6/(S/V) real V<0.5 l v V>10 l v films N Y M=M TRF *6/(S/V) real M FRF SML N N Y M SML 60 mg/kg M SML N Y M TRF SML Y N Y Non-compliant Compliant 7 Slide 8 References Hoekstra E.J., Petersen J.H., Bustos J. (2011) Guidance document on fat reduction factor, functional barrier concept, phthalates and primary aromatic amines. Publication Office of the European Union, Luxembourg, JRC Scientific and Technical Report, EUR EN Petersen J.H., Hoekstra E.J. (2011) Calculator for the correction of the experimental specific migration for comparison with the legislative limit in Regulation (EC) No 10/2011 on plastic food contact materials (version January 2012) 4 December

117 Slide 9 The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States 117

118 Lecture 8: Testing compliance for materials other than plastics Slide 1 Testing compliance for materials other than plastics Catherine Simoneau Slide 2 Overview Paper and board Other materials 118

119 Slide 3 Paper and board Manufactured from cellulose-based natural fibres both bleached and unbleached, from primary and recycled sources May contain functional additives and synthetic fibres and also other treatment agents and polymeric binders for organic and inorganic pigments May be coated and/or printed Slide 4 Paper and board Finland and The Netherlands have national requirements for paper and board Germany has established Recommendations concerning paper and board for different end-uses (e.g., baking and filter papers) For Member States without specific requirements for paper and board such materials are required to be safe National positive listings, EU Directives (such as the Plastics Directive, 2002/72/EC), EFSA evaluations Clearances in other jurisdictions (e.g., U.S. FDA) CoE Resolutions 119

120 Slide 5 CoE Resolution This Resolution applies to all food-contact paper including coated board and multi-layers Paper that is used in food-contact articles, but that is separated from the food by a functional barrier does not fall within the purview of the Resolution The Resolution also does not apply to non-woven materials, kitchen towels, napkins, and filter materials that are of a high base weight Slide 6 Paper and board CoE Res. AP (2002)1: Tech Doc No 1: Tech Doc No 2: Tech Doc No 3: Tech Doc No 4: Tech Doc No 5: General requirements List of substances (incomplete) Guidelines on test conditions and methods of analysis Guidelines for recycled fibres The CEPI Guide for GMP Practical Guide 120

121 Slide 7 Council of Europe Specifications Article 3 of the Framework Regulation Manufactured according to the CEPI GMP guide Suitable microbiological quality Should not release substances that have a microbiological effect Slide 8 Council of Europe Specifications Comply with restrictions assigned to the substances used in the manufacture of paper and board Inventory lists Cadmium, lead, mercury (compositional limit) Pentachlorophenol (purity requirement) Test conditions defined Compliance can be demonstrated by calculation 121

122 Slide 9 Recycled fibres Recycled fibres can be used (a) if it originates from specified qualities; (b) if they are subject to appropriate processing and cleaning (c) finished materials comply with the restrictions in the Resolution Guidelines on recycled fibres Slide 10 Paper and board Industry Guideline Document Developed by CEFIC, CEPI, CITPA, FPE Guideline-Food-Contact-%28CEPI-and-CI.pdf 122

123 Slide 11 Paper and board - methods Where available internationally recognised and validated methods should be used EN, ISO or equivalent If such standardised methods are not available, analytical methods with appropriate accuracy and precision may be used Slide 12 Paper and board - methods EN 645 Preparation of a cold water extract EN 647 Preparation of a hot water extract pren Preparation of an organic solvent extract EN Conditions for determination of migration from paper and board using modified polyphenylene oxide (MPPO) as simulant 123

124 Slide 13 Paper and board methods EN Determination of cadmium, lead and chromium in an aqueous extract EN Determination of mercury in an aqueous extract EN ISO Determination of pentachlorophenol in an aqueous extract EN 1104 Determination of transfer of antimicrobic constituents Slide 14 Paper and board methods EN 648 Determination of colour fastness of fluorescent whitened paper and board pren Determination of the migration of PAH-TEQ into food simulants pren Determination of phthalates in extract from paper and board 124

125 Slide 15 Paper and board methods CEN/TS Materials and articles in contact with foodstuffs Plastics substances subject to limitation - Part 13: Determination of 2,2-bis (4-hydroxyphenyl)propane (Bisphenol A) in food simulants Primary aromatic amines Michler s ketone & DEAB Benzophenone Slide 16 Migration into dry foods Cereals (9 months at ambient temperature) up to 45% migration observed Sugar (9 months at ambient temperature) no significant migration (< 1%) Brazil nuts (8 months at ambient temperature) up to 35% migration observed Powdered milk (8 months at ambient temperature) up to 100% migration observed 125

126 Slide 17 Migration into Tenax EN Conditions for determination of migration from paper and board using modified polyphenylene oxide (MPPO) as simulant Slide 18 How may migration into dry foods take place? Mechanism 1 dependent on free oil in the foodstuff many foods classified as dry do contain sufficient oil to wet the plastic the oil from within the food may penetrate the plastic accelerating the migration process 126

127 Slide 19 How may migration into dry foods take place? Mechanism 2 Migration proposed to occur through the vapour phase Five stages of migration Step 1. Composition of the packaging Step 2. Mobility in the packaging material Step 3. Volatilisation ( jumping the gap ) Step 4. Absorption onto the food surface Step 5. Mobility in the food Slide 20 Migration from paper and board Migration of DIPN from paper and board Migration of phthalates from paper and board Migration of mineral hydrocarbons from waxed paper and recycled paper/baord 127

128 Slide 21 Declaration of Compliance Date of Declaration of Compliance Manufacturer Identity of the materials and articles Confirmation of Compliance with the aforementioned industry Guideline and Regulation (EC) No. 1935/2004 Slide 22 Biosafepaper In-vitro testing of a paper/board extract Use of correction factors Proposal by the paper and board industry 128

129 Slide 23 Standard methods y Other (Materials and articles in contact with foodstuffs) CEN/TS 14234:2002 Polymeric coatings on paper and board- Guide to the selection of conditions and test methods for overall migration CEN/TS 14235:2002 Polymeric coatings on metal substrates - Guide to the selection of conditions and test methods for overall migration CEN/TS 14577:2003 Plastics - Polymeric additives - Test method for the determination of the mass fraction of a polymeric additive that lies below 1000 Daltons EN 14481:2003 Test methods for the determination of fatty contact EN 14233:2002 Determination of temperature of plastics materials and articles at the plastics/food interface during microwave and conventional oven heating in order to select the appropriate temperature for migration testing Cookware Cookware - Domestic cookware for use on top of a stove, cooker or hob - CEN/TS :2005 Part 2: Further general requirements and specific requirements for ceramic, glass and glass ceramic cookware Tableware Materials and articles in contact with foodstuffs - Cutlery and table holloware - EN ISO :1997 Part 1: Requirements for cutlery for the preparation of food EN ISO :1997 Part 2: Requirements for gold-plated cutlery EN ISO :1997 Part 2: Requirements for stainless steel and silver-plated cutlery EN ISO :1997 Part 3: Requirements for silver-plated table and decorative holloware EN ISO :1997 Part 4: Requirements for gold-plated cutlery EN ISO :2004 Part 5: Specification for sharpness and edge retention test of cutlery EN ISO :2000 Part 6: Lightly silver plated table holloware protected by lacquer EN ISO :2000 Part 7: Specification for table cutlery made of silver, other precious metals and their alloys EN ISO :2000 Part 8: Specification for silver table and decorative holloware Slide 24 Standard methods Standard reference Title lacquers Materials and articles in contact with foodstuffs - Certain epoxy derivatives subject to limitation EN 15136:2006 Determination of BADGE, BFDGE and their hydroxy and chlorinated derivatives in food simulants EN 15137:2006 Determination of NOGE and its hydroxy and chlorinated derivatives Ceramics Ceramic ware, glass-ceramic ware and glass dinnerware in contact with food ISO :1999 Ware: Release of lead and cadmium Part 1: Test method ISO : 1999 Ware: Release of lead and cadmium -- Part 2: Permissible limits ISO : 2002 Cookware: Release of lead and cadmium -- Part 1: Method of test ISO : 2002 Cookware: Release of lead and cadmium -- Part 2: Permissible limits Cook and tableware Materials and articles in contact with foodstuffs - Silicate surfaces - EN :1995 Part 1: Determination of the release of lead and cadmium from ceramic ware EN :1995 Part 2: Determination of the release of lead and cadmium from silicate surfaces other than ceramic ware 129

130 Slide 25 Standard methods Standard reference Title Glass Glass hollowware in contact with food ISO : 2005, Release of lead and cadmium -- Part 1: Test method ISO : 2005, Release of lead and cadmium -- Part 2: Permissible limits Enamel Vitreous and porcelain enamels ISO , 2003, Release of lead and cadmium from enamelled ware in contact with food -- Part 1: Method of test ISO , 2003, Release of lead and cadmium from enamelled ware in contact with food -- Part 2: Permissible limits Slide 26 Coatings CEN Technical Specification 14235:2002 Polymeric coatings on metal substrates Guide to the selection of conditions and test methods for overall migration Approach followed to determine overall and specific migration Rules for plastics generally followed to demonstrate compliance with the Framework Regulation 130

131 Slide 27 Introduction: coatings Act as a barrier between the metal of the can and the food Protect the food from the metal Protect the metal from aggressive food ingredients Need to be chemically resistant during sterilisation processes and mechanically flexible enough to enable manufacture of the can Also need to be safe for contact with food and beverages Slide 28 Typical can coatings Epoxy-anhydride (EAH) Epoxy-phenolic (EPH) Organosol (ORG) Polyester-polyurethane (PEPU) Targeted analysis Analytical screening 131

132 Slide 29 Can coating components and treatments Ingredients may include: Resins, often epoxy- or polyester-based Cross linking agents, e.g. phenolic resins Catalysts Lubricants Wetting agents Solvents Sterilisation conditions Potential for these components, or their reaction and degradation products to migrate from the can coating into food Slide 30 Non-intentionally added substances NIAS Example polyester-polyurethane coating Targeted analysis Screening analysis 132

133 Slide 31 Analysis Analytical techniques used to assess the safety of existing and new coatings: GC-MS (headspace and liquid injection) HPLC-MS/MS (triple quad) HPLC-TOF-MS HPLC-FLD and DAD ICP-MS Slide 32 Targeted versus screening analysis Both approaches are important Methods developed and optimised in different ways Targeted analysis Very specific conditions can be developed for one (or a few related) compound(s) Screening analysis Optimisation has to be a compromise because you don t know what you are looking for 133

134 Slide 33 Screening analysis Screening test protocol is applicable to all coating types Protocol requires a range of analytical instrumentation as well as knowledge and experience of typical can coating formulations Slide 34 GC-MS Headspace GC-MS analysis for volatile compounds Mass spectral reference libraries Concentrations estimated relative to internal standards No substances detected above the detection limit GC-MS analysis of solvent extracts for semi-volatile compounds Mass spectral reference libraries Concentrations estimated relative to internal standards Surfactants Plasticisers 134

135 Slide 35 GC-MS Full scan EI mass spectrum Abundance Typical of a PET oligomer Average of to min.: (-) m/z--> Slide 36 LC-TOF-MS < 3 ppm mass accuracy for confident identification Excellent mass resolution distinguishes compounds of interest from interferences 3-4 orders of magnitude dynamic range Automated delivery of reference standard maximises mass accuracy Fast scanning compatible with high-throughput screening 135

136 Slide 37 LC-TOF-MS analysis TIC Mass accurate to within 3 ppm Intensity x 10 4, counts [M+NH 4 ] m/z, amu [M+Na] amu 5 amu 16 amu [M+H] [M+K] Software predicts molecular formula Working with industry each potential migrant can be identified Slide 38 Screening summary Article 3 of the EU Framework Regulation Chemical migration from food packaging materials should not endanger human health Both targeted and screening analysis are required to support risk assessment for testing FCM 136

137 Slide 39 Printing inks Commission Regulation (EC) No 2023/2006 on GMP, Annex I specifically deals with printing inks Swiss Ordinance German recommendations Photoinitiators e.g. benzophenone, ITX Set-off Slide 40 Other Rubber Silicones Polymerisation aids Crystal glass Cork Ion exchange resins Colourants Council of Europe Resolutions 137

138 Slide 41 Cookware and tableware Coatings on metal substrates Same approaches as coatings applied to cans Perfluoro- compounds Metals and alloys Council of Europe Resolution Slide 42 CoE Guidelines on Metals and Alloys The following metallic materials are covered by the Guidelines: Aluminium, Chromium, Copper, Iron, Lead, Manganese, Nickel, Silver, Tin, Titanium, Zinc, stainless steel and other alloys The Guidelines also cover the below listed metals which may be present as impurities in some metallic materials and then migrate: Cadmium, Cobalt and Mercury Recommendations for each element and impurity listed 138

139 Slide 43 Slide

140 Slide 45 The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States 140

141 Lecture 9: Testing for dry foods tests with the new simulant Slide 1 Testing for dry foods- tests with the new simulant Tenax Natalia Jakubowska Slide 2 TENAX - registered trademark for poly(2,6-diphenyl-p-phenylene oxide) (MPPO Tenax TA); - particle size mesh; - pore size 200 nm; - high molecular weight, to dalton; - very high temperature stability T max = 350 C; - high surface area and low specific mass, 0.25 g/cm 3 ; - porous polymer which efficiently traps volatiles and semi-volatiles; - powdery and lightweight and is readily blown about by air currents

142 Slide 3 TENAX types: Tenax GR Tenax GC replaced by: Tenax TA Slide 4 Tenax GR www. sisweb.com 142

143 Slide 5 Tenax TA www. sisweb.com Slide 6 TENAX Recognized by the European Commission in legislation 2nd amendment of Directive 82/711/EEC for testing plastics as a substitute test medium for fatty food; Directive 97/48/EEC as a substitute for olive oil for high temperatures; Regulation (EU) No 10/2011 Food simulant E for testing specific migration into dry foodstuffs

144 Slide 7 TENAX in Regulation (EU) No 10/2011 Annex III 2. General assignment of food simulants to foods Food simulant E is assigned for testing specific migration into dry foods. 3. Specific assignment of food simulants to foods for migration testing of materials and articles not yet in contact with food Table 2. food category specific assignment of food simulants 7 Slide 8 Regulation (EU) No 10/2011 Table 2. food category specific assignment of food simulants Ref. no. Description of food Food simulants E Cereals, cereal products, pastry, biscuits, cakes and other bakers wares Starches Cereals, unprocessed, puffed, in flakes (including popcorn, corn flakes and the like) Cereal flour and meal Dry pasta e.g. macaroni, spaghetti and similar products and fresh pasta Pastry, biscuits, cakes, bread, and other bakers wares, dry: A. With fatty substances on the surface B. Other Pastry, cakes, bread, dough and other bakers wares, fresh: A. With fatty substances on the surface X X X X X X B. Other 8 144

145 Slide 9 Table 2. food category specific assignment of food simulants Ref. no. Description of food Food simulants E Chocolate, sugar and products thereof Confectionery products A. In solid form: I. With fatty substances on the surface II. Other X Sugar and sugar products A. In solid form: crystal or powder X Fruit, vegetables and producs thereof Processed fruit: A. Dried or dehydrated fruits, whole, sliced, flour or powder X Nuts (peanuts, chestnuts, almonds, hazelnuts,, walnuts, pine kernels and others): A. Shelled, dried, flaked or powdered X X B. Shelled and roasted 9 Slide 10 Table 2. food category specific assignment of food simulants Ref. no. Description of food Food simulants E Processed vegetables: A. Dried or dehydrated vegetables whole, sliced or in thhe form of flour or X powder Animal products and eggs Whole eggs, egg yolk, egg white X A. Powdered or dried or frozen Milk products B. Milk poder including infant formula (based on whole milk powder) Cheeses: A. Whole, with not edible rind Miscellaneous products Preparations for soups, broths, sauces, in liquid, solid or powder form (extracts, concentrates); homogenised composite food preparations, prepared dishes including yeast and raising agents A. Powdered or dried: I. With fatty character II. Other X X X 145

146 Slide 11 Table 2. food category specific assignment of food simulants Ref. no. Description of food Food simulants E Sandwiches, toasted bread pizza and the like containing and kind of foodstuff A. With fatty substances on the surface X B. Other Dried foods: A. With fatty substances on the surface B. Other Frozen and deep-frozen foods Coffee, whether or not roasted, decaffeinated or soluble, coffee substitutes, granulated or powdered Aromatic herbs and other herbs such as camomile, mallow, mint, tea, lime blossom and others Spices and seasonings in the natural state such as cinnamon, cloves, powdered mustard, pepper, vanilla, saffron, salt and otther X X X X X 11 Slide 12 Regulation (EU) No 10/2011 Annex III 3.2 Substitute test for OM7 with food simulant D2 In case it is technically NOT feasible to perform OM 7 (2h at 175 C ) with food simulant D2 (vegetable oil) the test can be replaced by test OM 8 or OM 9. Both test conditions described under the respective test shall be performed with a new test sample

147 Slide 13 CEN methods 13 Slide 14 EN ; 2002 Materials and articles in contact with foodstuffs Plastics Part 13: Test methods for overall migration at high temperatures Method B Adsorption by modified polyphenylene oxide - for test conditions from 100 C and maximum temperature applicable is 175 C; - heating take place in the oven even if the samples are for use in a microwave oven; - extraction are made with diethyl ether; - residue remaining is determined gravimetrically;

148 Slide 15 Cleaning procedure Prior to its first use the MPPO shall be purified by soxhlet extraction, using diethyl ether as follows: - Place the MPPO in a soxhlet cartridge and extract for 6h with diethyl ether; - Spread the MPPO in a Petri dish of a suitable diameter and place the dish in a fumehude; - Allow the ether to evaporate while frequently mixing with a glass rod; - Place the dish in an oven at 160 C for 6h; - After heating store the MPPO in closed conical flask. 15 Slide 16 Cleaning procedure -Notes Note1. Heating of MPPO saturated with diethyl ether can be explosive. Therefore, it should be ensured that diethyl ether is completely evaporated before drying at 160 C; Note 2. MPPO cleaned in this way can be used repeatedly; Note 3. When drying MPPO, the oven should be set to low force and the MPPO should be cover by the dish to prevent the MPPO from blowing about; Note 4. The diethyl ether is often stabilized by BHT

149 Slide 17 Exposure to MPPO (triplicate): - inner diameter of the glass ring should be taken into account (effective contact area); - to cover the food contact surface sufficiently, 4 g MPPO per 1 dm 2 of surface area of the test specimen is required; Note1. When the test sample is placed into the oven the time required to reach the intended temperature can be significant. Therefore it can be necessary to include a procedure to control of the time and temperature in order to achieve reproducible and repeatable results; 17 Slide 18 Exposure to MPPO: Note 2. In the case of the articles of irregular geometry and with not flat areas. Possible solutions are to cut the appropriate parts and mix with MPPO using the conventional mass of MPPO (4 g/dm 2 ) or if necessary, higher amount of MPPO should be used to ensure complete contact between the test specimen and MPPO. For the blank determination, take an empty Petri dish and place inside the same amount of MPPO (without test specimen). Remove the test specimen from the oven and allow them to cool down to room temperature without removing the glass covers (takes approximately 0.5h)

150 Slide 19 Determination of the migrating substances: - Transfer the MPPO into the Erlenmeyer flask with the aid of the funnel (use the brush when it s necessary); - Calculate by reference to the Table the volume of diethyl ether needed for extraction Mass of the MPPO Volume of Volume of Volume of diethylether for 1 st diethylether for 2 nd diethylether for 3 rd extraction extraction extraction Slide 20 Determination of the migrating substances: - Pour the diethyl ether through the funnel into the Erlenmeyer flask and shake manually 1 min., - Allow the Erlenmeyer flask and its content to stand for 1 min, without shaking; - Place a folded filter into the funnel and insert the funnel into the vial. During the extraction of MPPO the solvent is decant from the extracted MPPO (some of the solvent is absorb by the Tenax); - Repeat this extraction procedure twice; -Rinsethe filter with 10 ml diethyl ether; -Concentratethe combine diethyl ether solutions to approximately 5ml, first using rotary vapour then gently nitrogen flow;

151 Slide 21 Determination of the migrating substances: -Weighthe 10 ml vials with accuracy of ± 0.1 mg; - Transfer each of the concentrated extract into the vials using the dropping pipette and include a rinsing step using 5 ml of diethyl ether; -Evaporatethe concentrates to dryness using the stream of the nitrogen (around 30 min.), until constant weight has been achieved (when the weight difference is equal or smaller than 0.5 mg -monitored every 5 min.); - Determine the mass of the residue by subtracting the original mass of the vial from the stable mass of the vial and residue; 21 Slide 22 Expression of results: M=(m a -m b )/s M is the mass of the migrated substances adsorbed onto MPPO from the test specimen, in milligrams per square decimeter; m a is the mass of the residue from the MPPO that had been in contact with the test specimen; m b is the mass of the residue from the MPPO that not had been in contact with the test specimen; s is the surface area of the test specimen that was in contact with MPPO, in square decimeters

152 Slide 23 DIN EN 14338; 2004 Paper and board intended to come into contact with foodstuffs Conditions for determination of migration from paper and board using modified polyphenylene oxide (MPPO) as a simulant - migration of specific volatile and semivolatile substances from paper and board intended to come in contact with dry, not fatty foodstuffs for backing purpose and in the last case can be seen as a substitute simulant for fatty contact; - maximum temperature applicable is 175 C; - heating take place in the oven even if the samples are for use in a microwave oven; - extraction are made with organic solvent depending on the used specific analytical method; -in this extract the analysis for the desired components is possible; 23 Slide 24 Cleaning procedure Extracting using acetone is obligatory for complete purification of the MPPO prior to first use as follows: - Place the MPPO in a soxhlet cartridge and extract for 6h with acetone; - Spread the MPPO in a Petri dish of a suitable diameter and place the dish in a fumehude; - Allow the solvent to evaporate while frequently mixing with a glass rod; - Place the dish in an oven at 160 C for 6h; - After heating store the MPPO in closed Erlenmeyer flask

153 Slide 25 Cleaning procedure -Notes Note 1. MPPO can be used repeatedly if cleaned in this way between uses; Note 2. When drying MPPO in a forced air oven the dishes should be covered to prevent the MPPO from blowing about 25 Slide 26 Exposure to MPPO (duplicate): Paper - to cover the food contact surface sufficiently, 4 g MPPO per 1dm 2 of surface area of the test specimen is required; Note 1.Cell according to EN or Petri dish without the glass ring Note 2. Bed of MPPO should cover all test specimen, to uniform depth when the test sample is placed into the oven

154 Slide 27 Exposure to MPPO: Note 3. Petri dish should be placed into preheated incubator and start the time when the temperature has recovered to a temperature within the permitted tolerance for the test temperature; For the blank determination, take an empty Petri dish and place inside the same amount of MPPO (without test specimen). Remove the test specimen from the oven and allow them to cool down to room temperature without removing the glass covers (takes approximately 0.5h). 27 Slide 28 Extraction of the MPPO: - Transfer the MPPO into the Erlenmeyer flask with the aid of the funnel (use the spoon when it s necessary); - Pour 20 ml of the organic solvent through the funnel without the frit into the Erlenmeyer flask and shake manually for 1 min.; - Allow the Erlenmeyer flask and its content to stand for 5 min, without shaking; - Decant the solvent from MPPO into 50 ml volumetric flask; - Repeat the extraction using 20 ml of solvent; - Rinse the filter with the organic solvent and fill to the mark; - Aliquots can be used for further analysis

155 Slide 29 SOP proposed by JRC for ILC BHT, BP, DiBP, DEHA and DINCH in TENAX and migration experiments from spiked film Used for: -spiked Tenax - Tenax after migration 10 days 60 C Slide 30 Cleaning procedure according to DIN EN h soxhlet extraction using acetone Exposure to Tenax (4 replicates - test specimen): - migration conditions: 10 days 60 C; - to cover the food contact surface sufficiently, 1 g MPPO per 0.15 dm 2 of surface area; higher amount of Tenax were used to ensure complete contact between the test specimen and Tenax ;

156 Slide 31 Migration test sample preparation: - Place LDPE foil into the Petri dish; - Place the glass O-ring in the middle of the LDPE foil; - Weight 1.0 ± 0.1 g of the clean MPPO and put inside the O-ring; - Close the Petri dish; - Shake gently the closed Petri dish to cover all the LDPE foil; - Wrap the Petri dish by aluminum foil carefully to keep the LDPE foil surface covered by Tenax ; 31 Slide 32 Migration test sample preparation: - Put the Petri dish inside the oven at 60 C for 10 days; - After migration test take out the Petri dish from the oven; - Transfer carefully the Tenax into 40 ml vial or the Erlenmeyer flask using funnel. 156

157 Slide 33 Preparation of the calibration curve in Tenax : - Weight 1.0 g of clean MPPO in 40 ml vials or Erlenmeyer flasks; -Spike the Tenax following the SOP; -Extract the Tenax ; -Use the Tenax without the spiking as a blank. Slide 34 Extraction of the Tenax : - Transfer 1.0 g of the Tenax (or all the Tenax from the Petri dish after migration) into the 40 ml vial; - Add 20 ml of extraction solution (Hexane ppm of BBP); - Shake manually for 1 min; - Leave it for 5 min without shaking; - Insert the funnel with the filter into a new 40mL vial; 157

158 Slide 35 Extraction of the Tenax : - Decant the hexane from the Tenax through the filter into the new vial; - Repeat extraction once again; - Collect the extracts; - Evaporate the hexane extract under the nitrogen to around 5 ml; - Inject the concentrated extract into GC-MS. Slide 36 Additional information: SOP for spiking the Tenax: - define weight of the cleaned Tenax was weighted and transferred into the 10 L round bottom flask; - 1 L of the spiking solution in pentane was add to the Tenax ; - The flask was rinsed by pentane and all liquid was collected in the round bottom flask; - The flask was closed and the Tenax was mixed continuously for 2 hours; - The flask was open and the Tenax was mixed till the complete evaporation of the pentane. 158

159 Slide 37 Additional information: SOP for spiking the LDPE foil: - the LDPE foil (size: 30x100 cm) was placed into the reaction chamber; - the foil was rolled and did not touch the chamber walls; - the chamber was filled by the ethanol spiking solution to cover up the LDPE foil; - the reaction chamber was placed into the oven at 60 C for 2 days; - after the exposure time the foil was taken out from the chamber and rinsed carefully with the fresh ethanol, dried and cut into the discs. Slide 38 Thank you very much attention!

160 Slide 39 The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States 160

161 Lecture 10: Method validation requirement and quality assurance plans Slide 1 Method validation requirements and quality assurance plans Catherine Simoneau Slide 2 Overview Use of in-house test procedures validation requirements (how do we know that a method is acceptable ) Quality assurance and quality control plans for laboratories Availability of proficiency testing schemes and reference materials 161

162 Slide 3 Official controls Guarantee the safety of foods and ensure their free circulation in the EU Risk assessment = exposure assessment + hazard characterisation (toxicology) How: Harmonise performance of national laboratories, of their methods: more reliable results Mutual recognition of results Measured Once, trusted everywhere Better consumer protection =Boost trust Risk management (RM)= accounting and addressing (SANCO) Communication = transparency interactive process Official controls = RASFF + implementation/ enforcement of RM Consumer protection and trust EU-RL - NRLs Slide 4 Guidelines on method performance Twenty three CEN standards/technical Specifications > 2000 authorised substances for plastics EU-RL Guidelines Guidelines for performance criteria and validation procedures 162

163 Slide 5 Quality assurance QA) Quality assurance with accreditation ISO Quality assurance with method performance demonstration and analytical results evaluation Quality assurance with Laboratory proficiency testing Slide 6 Quality assurance (QA) A good quality assurance system can show at anytime The justness The uncertainty of analytical results A good quality assurance system needs Clear organization and responsibilities Criteria when what to decide and by whom Clear working procedures and arrangements To be understandable for the person who is working with it ISO Accreditation based QA 163

164 Slide 7 Need for accreditation Why accreditation? Universal recognition Accreditation proves the quality of a laboratory Gives third party confidence What is accreditation? A team of experts comes and visits the laboratory to verify conformity to ISO If conform to ISO the assessing body attests conformity through a certificate Accreditation is tested every year EU-RL and NRLs: MUST be accredited in 882/2004 OFFC Slide 8 Accreditation Accreditation bodies around the world 164

165 Slide 9 Approaches Accreditation of a laboratory Accreditation of a method Accreditation by flexible scope Slide 10 Need for traceability Accreditation obliges to prove (criterion 5.6) Traceability Line controls Traceability Mass pieces, thermometers, critical instruments, etc need to be calibrated BY CERTIFIED INSTITUTE Line controls The PERIODICAL analysis of a sample of known quantity in a know medium (e.g. oil, water, etc) Continues check of laboratory quality Can always prove laboratory quality 165

166 Slide 11 Need for control samples 1st, 2nd, 3rd line control 1st line: matrix and quantity are known by operator 2nd line: matrix and quantity are unknown by operator but known in the lab 3rd line: quantity is unknown in the laboratory (provided by an external lab e.g. Proficiency test) MATRIX = MEDIUM (OIL, WATER) Slide 12 Need for control samples Minimum of 2 line controls should be operational Preference for 1st and 3rd line 2nd line only when no 3rd line is available Frequency of line controls: depending on use of method 1st line: usually every time the method is used 2nd lines: usually once every 3 months 3rd line: usually once or twice a year (depends on availability and/or stability of samples) 166

167 Slide 13 How can these controls be achieved n in practice? 1st line: possibilities Common sample Spiked sample Reference sample 2nd line: possibilities Same as 1st line but: Colleague or another department of lab makes sample with known quantity Repeating the analysis of an earlier sample Repeating the analysis of a proficiency testing sample Slide 14 How can these controls be achieved n in practice? 3rd line possibilities Participation in Proficiency testing (PT) scheme 167

168 Slide 15 QA method performance Slide 16 Method Performance -Regulation OFFC Hierarchy of methods Community methods (laid down in legislation) Internationally recognised methods, e.g. CEN-methods Method fit for the purpose or developed in accordance with scientific protocols Single laboratory validated methods 168

169 Slide 17 Characterisation of methods of analysis Accuracy; Applicability matrix and concentration range Limit of detection Limit of determination / quantification Precision Repeatability Reproducibility Recovery Selectivity Sensitivity Linearity Measurement uncertainty Other criteria that may be selected as required Slide 18 Precision data: how? Collaborative trial using international protocols (e.g. ISO 5725: 1994, I UPAC International Harmonised Protocol) If not, then single laboratory validation e.g. IUPAC Harmonised Guidelines OFFC gives parameters and some specifics It also leaves open some practical implementation of the requirements Let s look at some of these requirements. 169

170 Slide 19 Precision parameters Relationship between R, RL and r Repeatability, r run labs lab Reproducibility within-lab, RL Reproducibility, R Slide 20 Bias Trueness, (bias, accuracy of the mean) The closeness of agreement between the average value obtained from a large series of test results and an accepted reference value Use Certified Reference Materials (CRMs) or recovery experiment Recovery Proportion of the amount of analyte, present in the analytical portion of the test material, which is extracted and presented for measurement ISO

171 0,20 0,15 0,10 0,05 0,00-0,20-0,15-0,10-0,05 0,00 0,05 0,10 0,15 0,20-0,05-0,10-0,15-0,20 0,20 0,15 0,10 0,05 0,00-0,20-0,15-0,10-0,05 0,00 0,05 0,10 0,15 0,20-0,05-0,10-0,15-0,20 0,20 0,15 0,10 0,05 0,00-0,20-0,15-0,10-0,05 0,00 0,05 0,10 0,15 0,20-0,05-0,10-0,15 Slide 21 Measurement Uncertainty Parameter charactering the dispersion of the values of results of a measurement. Different approaches AOAC EURACHEM s δ δ s Random errors (sdev) Systematic errors (bias) -0,20 Slide 22 Importance of method performance and criteria in compliance assessment Non-compliant Compliant Eurachem/CITAC Guide, 2007 Slide

172 Use of Measurement Uncertainty (MU) in compliance assessment Rules to estimate MU used by enforcement authorities Especially for empirical methods which are often used in case of FCM. Harmonised implementation by authority's Commission Regulation (EC) No 882/2004 Needs: Proficiency trials and CRMs Specifications for maximum MU accepted as fit-for-purpose Way of reporting results Whether analytical results are (non-)recovery corrected Slide 24 Proficiency testing Slide

173 What is proficiency testing? An interlaboratory system for the regular testing of the accuracy that the participant laboratories can achieve Purpose To help laboratories detect and cure any unacceptably large inaccuracies in their reported results Ensures results are meaningful Quality assurance Linked to maintaining ISO accreditation Contributes/enhances laboratory reputation Slide 26 Proficiency testing (PT) Analysis of same samples by multiple laboratories and statistical evaluation of the results Valid statistical best estimate of the true value Should measure typical performance rather than highest capability Can help to: Improve or maintain high quality in laboratory performance. Indicate inadequacies in methodologies, reagents, equipment and performance. Stimulate education and self- of laboratory personnel 173

174 Slide 27 PT- a duty for official controls A control laboratory has requirements to be accredited e.g Accreditation checks the process 5.0 A control laboratory should also use PTs as self check on 4.0 performance vs. others z-score Laboratory Number Slide 28 Organisation of proficiency testing (PT) 174

175 Slide 29 Test material requirements Relevant test material with relevant analyte / concentration combinations As close as possible to the materials being regularly analysed Not always easy to find naturally contaminated materials Confidence in analyte stability Confidence in the homogeneity of the test material Slide 30 PT schemes: very few for FCM testing FAPAS (UKAS accredited) VWA KIWA TNO RIKILT LGC More info: EPTIS database lists PT schemes (PTS) operated in Europe, the Americas and in Australia. The focus is on the field of testing; EU-RL organised inter-laboratory trials 175

176 Slide 31 Needs; RMs and PTs (Certified) Reference Materials Needed for PTs Needed for method validation (included materials to include t/t) CRMs only available for overall migration PTs: best way to self check performance vs. others Lack of PT schemes for food contact materials FAPAS (UKAS accredited) Slide 32 FAPAS Rounds Series 11 OM into an aquous simulant OM into olive oil Series 12 Phthalates in simulant Melamine in simulant PAAs in simulant Bisphenol A in simulant Photonitiators 176

177 Slide 33 Interlaboratory exercises The ability for laboratories to provide method independent reliable results (Proficiency testing, PT) The ability of the method of analysis to produce reliable results (Method validation) Parameters are set out in Regulation 882/2004 on official feed and food controls (LOD, LOQ, repeatability, reproducibility, precision, accuracy etc) EU-RL organised exercises Slide 34 Conclusions Laboratories must be accredited or follow documented quality assurance Proficiency testing to prove that laboratories are performance Method performance check (or validation) to prove a method is suitable Mutual recognition of measurement data is only possible under these circumstances 177

178 Slide 35 Conclusions Importance of mutual recognition of measurement data Foster confidence in certificates Promote trade Foster acceptance of accredited laboratory data Avoid unecessary duplication of efforts Slide 36 The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States 178

179 Satisfaction survey and customer feedback This training was the subject of a customer satisfaction survey to have a feedback on the services provided by our Unit towards this initiative. The customer satisfaction survey was carried out following the Unit procedure, using the pre approved form. The questionnaire was submitted to the 14 participants of the workshop on 6 7 November replies were received anonymously upon leaving, i.e. from all 14 participants (Annex 3). Feedback received from the participants was very positive. Results from this evaluation resulted in around 100% of satisfaction (good and very good). Remarks highlighted the complexity of the field and wishes for further training that could include hands on laboratory demonstrations. In addition 8 personal e mails of thank you and appreciation were received, showing how useful the training was beyond the survey conducted. The e mails in particular requested to be informed of further initiatives, thus highlighting an intention of making use of the knowledge acquired within this initiative. This respond to the mandate of the EURL FCM towards third countries this event will be also briefed to National Reference Laboratories. Excerpts (not exhaustive) of appreciation received in further spontaneous e mails Thanks for the training course, it was very interesting and formative. My colleague and I hope to participate to other workshop like this one Elena Giacomazzi, Laboratory Manager, Vailati First of all, I really want to thank you for invitation to the workshop about FCM testing on 6 7/11/2012 in Ispra. I am too satisfied by that workshop. It was great to be in JRC. Hopefully I wish to be there again with much more detailed workshops, also laboratory training. I would love be in touch with JRC. As a result of past workshop I learnt so much about FCM testing and EC regulations Ali Bahadir Celik, MSc. Food Engineer, Ministry of Food, Agriculture and Livestock, Istanbul Food Control Lab. THANK YOU all for a interesting and very useful training!. Please send my thanks to all the others who made our stay so meaningful and pleasant. Susanne Ekroth, Head of the National Reference Laboratory for Food Contact Materials, Sweden We had a nice workshop at JRC. I think it was very useful and timely workshop for us all. I would like to express my thanks to you and your team for organizing such a good informative workshop. This workshop was the result of many years of experience and hard work. I congratulate you and your team. There are several areas that we could cooperate in the coming months which will be very beneficial for all the parties involved. I am looking forward to this cooperation. Dr.Fatih YILDIZ, Professor/Director, Middle East Technical University, Department of Food Engineering, Ankara Turkey Thank you for so informative workshop and 2 very nice days at JCR in Ispra.. Ivan.Mijatovic, Regulatory affair specialist, Rexam, UK Thank you very much for the workshop provided last week. It was a beneficial and fruitful one. Gerald Chung, scientific officer, Health Science Authority, Singapore 179

180 Acknowledgments Part of these slides were developed together with Emma Bradley (FERA, UK) and for modelling from Rainer Brandsch (MDCTec). They are gratefully acknowledged. 180

181 Annex 1 - Highlights photos from the training 181

182 Annex 2 - Participants NP: did not participate 182

183 Annex 3 - Customer satisfaction survey 183

184 Customer satisfaction survey results Programme Objectives Contents, quality of presentations Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Discussion time / interaction between participants Workshops / sub sessions Balance between sessions Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Note on balance between session: one presentation on legislation ran overtime due to Q&A; the time which was made up in day two. Speakers performance Supporting material Provision of additional resources (useful links, downloads, contacts) Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Organisation Location Side events (lunch, coffee break) Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Online registration Overall evaluation of the event Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer Very good Good Satisfactory Could be improved Unsatisfactory N/A No answer 184

185 European Commission EUR Joint Research Centre Institute for Health and Consumer Protection Title: Enlargement and Integration Workshop: EU legislation and testing for the chemical safety of food contact material" Author(s): C. Simoneau, E. Hoekstra, N. Jakubowska Luxembourg: Publications Office of the European Union pp x 29.7 cm EUR Scientific and Technical Research series ISSN (online) ISBN (pdf) doi: /67212 Abstract In the framework of the "Enlargement and Integration initiative", the European Commission Joint Research Centre (JRC) organised a training workshop focusing the latest EU Directives and legislative requirements for food contact materials (FCM), and details of the experimental procedures for compliance testing against the requirements. The workshop took place in Ispra on 6 7 November The list of topics covered included: EU Directives and legislative requirements for FCM including active and intelligent materials, requirements for compliance for imports, Testing for compliance for plastics including modelling as well as for materials other than plastics, testing specific migration for dry foods with the new simulant in the newly established Regulation 10/2011, and method validation, requirements for quality assurance and proficiency testing programmes. This training also included a laboratory visit and was the subject of a satisfaction survey. The outlook of the training showed not only a significant impact for the participants as shown by the satisfaction survey but also by the spontaneous e mails also received as follow up. The feedback of the training also showed the necessity and wishes for further trainings and collaborations in this field. 185

186 LB-NA EN-N As the Commission s in-house science service, the Joint Research Centre s mission is to provide EU policies with independent, evidence-based scientific and technical support throughout the whole policy cycle. Working in close cooperation with policy Directorates-General, the JRC addresses key societal challenges while stimulating innovation through developing new standards, methods and tools, and sharing and transferring its know-how to the Member States and international community. Key policy areas include: environment and climate change; energy and transport; agriculture and food security; health and consumer protection; information society and digital agenda; safety and security including nuclear; all supported through a cross-cutting and multi-disciplinary approach. 186