Enlargement and Integration Workshop...2 Migration (mg/dm) no fat 10% fat 20% fat 30% fat 50% fat...

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

Transcript of Enlargement and Integration Workshop...2 Migration (mg/dm) no fat 10% fat 20% fat 30% fat 50% fat...

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    Report EUR 25599EN

    Enlargement and Integration Workshop

    2 0 1 2

    C. Simoneau, E. Hoekstra, N. Jakubowska

    “EU legislation and testing for the chemical testing of food contact materials” Ispra, 6-7 November 2012

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    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, 21027 Ispra (VA), Italy E-mail: [email protected] Tel.: +39 0332 78 5889 Fax: +39 0332 78 5707 http://ihcp.jrc.ec.europa.eu/ http://www.jrc.ec.europa.eu/ 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 (*): 00 800 6 7 8 9 10 11 (*) Certain mobile telephone operators do not allow access to 00 800 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 http://europa.eu/. JRC76765 EUR 25599 EN ISBN 978‐92‐79‐27392‐6  (pdf) ISSN 1831‐9424 (online) doi:10.2788/67212 Luxembourg: Publications Office of the European Union, 2012 © European Union, 2012 Reproduction is authorised provided the source is acknowledged. Printed in Italy

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    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 2012. 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.   

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    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............................. 23 Lecture 3: Procedure and testing requirements for importing FCM in the EU. ...... 58 Lecture 4: Active and intelligent packaging............................................................................ 65 Lecture 5: Testing compliance: migration testing for plastics........................................ 76 Lecture 6: Migration modelling for compliance testing of plastic FCM ................... 104 Lecture 7: Correction factors of experimentally determined specific migration 113 Lecture 8: Testing compliance for materials other than plastics ............................... 118 Lecture 9: Testing for dry foods – tests with the new simulant.................................. 141 Lecture 10: Method validation requirement and quality assurance plans ............ 161

    Satisfaction survey and customer feedback ............................................................................. 179 Annex 1 ‐ Highlights photos from the training........................................................................ 181 Annex 2 ‐ Participants ........................................................................................................................ 182 Annex 3 ‐ Customer satisfaction survey ..................................................................................... 183

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    Programme   

    Workshop  "EU legislation and testing for the chemical safety of food contact material" 

     Updated AGENDA 0607.11.2012 

       

    06/11/2012  08:30  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  07/11/2012    09:00    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 12:3014:00  Lunch 14:00‐15:00  Testing kitchenware and worked examples (C. Simoneau) 

    Q&A, wrap up session   ±16:00  closure (depending on travel schemes)

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    Presentations

    Lecture 1: Introduction to food contact materials  

    Slide 1 

     

    Science for a healthier life

    Institute for Health and Consumer Protection

      

     

     

    Slide 2 

     

    Introduction to Food Contact Materials

    Catherine Simoneau

      

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    Slide 3 

     

    Food contact materials • Food processing equipment, tubing, conveyor belts, etc

    • Packagingmaterials

    • 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

      

     

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    Slide 5 

     

    Package FoodsINTERACTION

      

     

     

     

    Slide 6 

     

    Innovation to assure quality of food and to extend its shelf-

    life

    Materials and containers with

    specific technical characteristics

    Interest of all official

    institutions

    Development of control techniques to assure quality and safety of

    packaged food

    Safety in development and innovation

    New materials (production and

    design)

      

     

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    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

      

     

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    Slide 9 

     

    Types of food packaging materialsConventional: • Plastics,• Regenerated cellulose, • Paper and board, • Glass and ceramics, • Elastomers, • Metals, • Wood, textile, waxes etc.• Recycled

    Biobased: made from renewable sourcesActive: 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 sub-microscopic processes

    May impact food in two ways• Food safety – migration of harmful substances• Food quality – migration of substances which impart taint or odour

    Migration FoodPackaging

      

     

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    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 

     

    Packaging

    Impermeable materials:- glass & ceramics- metals & alloys

    xyz

    Food

    Depiction of chemical migration from an impermeable material

    The nature of the FCM

      

     

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    Slide 13 

     

    Packaging

    Permeable materials: - plastics- rubber & silicone- coatings

    xy

    z

    Food

    Depiction of chemical migration from a permeable material

    The nature of the FCM

      

     

     

     

    Slide 14 

     

    Packaging

    Porous materials:e.g. paper and board

    x

    z

    Food

    y

    Depiction of chemical migration from a porous material

    The nature of the FCM

      

     

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    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 

     

    M.P Steven, Journal of Chemical Education, 1993, 444

    Typical additives for plastics

    StabilisersUV absorbersPreservativesOptical brightenersFoaming agentsRelease agentsetc

    Anti-oxidantsPlasticisersLubricantsEmulsifiersFillersFlame retardantsImpact modifiers

      

     

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    Slide 17 

     

    Irganox 1330

    Irganox 1010Irganox 1076

    BHTBis(2-ethylhexyl) phthalate = DEHP

    Bis(2-ethylhexyl) adipate = DEHA

    Acetyl tributyl citrate = ATBC

    Potential migrants from plastics

    plasticisers (up to 40%) antioxidants (up to 0.5%)

    Chimassorb 81

      

     

     

     

    Slide 18 

     

    0

    0.2

    0.4

    0.6

    0.8

    1

    1.2

    1.4

    0 50 100 150 200Time (days)

    Mig

    ratio

    n in

    to fo

    od (m

    g/kg

    )

    200 Da additive500 Da additive1000 Da additive

    The nature of the migrating substance

      

     

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    Slide 19 

     

    0.0

    0.5

    1.0

    1.5

    2.0

    2.5

    3.0

    0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5

    Time (days)

    Mig

    ratio

    n (m

    g/dm

    2 )

    no fat10% fat20% fat30% fat50% fat

    High fat = low caprolactam migration

    Low fat = high caprolactam migration

    The nature of the foodstuff

      

     

     

     

    Slide 20 

     

    • Interaction between food and packaging

    • Direct versus indirect contact

    • Point or continuous contact

    The nature of the contact

      

     

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    Slide 21 

     

    0

    2

    4

    6

    8

    10

    12

    0 1 2 3 4 5 6 7 8 9 10

    Time (days)

    MIg

    ratio

    n (m

    g/kg

    )

    15°C30°C40°C

    Time and temperature

      

     

     

     

    Slide 22 

     

    Potential migrants from printing inks

    Binders (monomers)

    Colourants and pigments

    Solvents to dissolve pigments and resins

    Catalysts or initiators of UV curing

      

     

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    Slide 23 

     

    Potential migrants from paper and board

    INGREDIENTS SUBSTANCES MIGRATING

    Chlorine bleaches chlorophenols formation

    Sizing agents waxes, starch derivatives

    (strength of paper when wet)

    Fat repellents fluoroalkyl polymers

    Volatiles aldehydes, ketones

      

     

     

     

    Slide 24 

     

    Potential migrants from (coated) metal

    Epoxy and epoxy-phenolicsBADGE, BFDGE from the epoxy

    resin – hydroxy and chlorinated derivates

    Vinyl systemsvinyl chloride and vinyl acetate

    Lacquers

    Tinplate for cans Tin, chromiumTin

      

     

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    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)

      

     

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    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

      

     

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    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

      

     

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    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

      

     

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    Slide 33 

     

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

    States

      

     

     

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    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

    www.jrc.ec.europa.eu

      

     

     

    Slide 2 

     

    EU legislationon food contactmaterials

      

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    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)

      

     

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    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 animals1973 – migration from PVC food packaging materials1973 – MAFF WG on VCM was established1974 – Clear link between angiosarcoma and occupational

    exposure of US workers1978 – Directive 78/142/EEC sets QM = 1 mg/kg and

    SML=ND (0.01 mg/kg)

      

     

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    Slide 7 

     

    + Coatings

    93/11/EECNitrosamines

    Monomers and

    additives2002/72/ECas amended

    Vinyl chloride

    78/142/EEC 80/766/EEC81/432/EEC

    Migration testing 82/711/EECas amended

    List of simulants85/572/EEC as amended

    BADGE/BFDGE/NOGE

    1895/2005/EC

    Reproduced with the kind permission of Annette Schaefer (DG-SANCO, European Commission)

    Recycled plastics(EC) No 282/2008

    Plasticisers in gaskets(EC) No 372/2007

    as amended

    Ceramics84/500/EEC as amended

    Plastics Elastomersand

    rubbers

    EU legislation

    Active and intelligent materials (EC) No 450/2009

    Regeneratedcellulose film 2007/42/EC

    Food contact materials (EC) No 1935/2004

    Good manufacturing practice (EC) No 2023/2006

      

     

     

     

    Slide 8 

     

    + Coatings

    93/11/EECNitrosamines

    Monomers and

    additives2002/72/ECas amended

    Vinyl chloride

    78/142/EEC 80/766/EEC81/432/EEC

    Migration testing 82/711/EECas amended

    List of simulants85/572/EEC as amended

    BADGE/BFDGE/NOGE

    1895/2005/EC

    Reproduced with the kind permission of Annette Schaefer (DG-SANCO, European Commission)

    Recycled plastics(EC) No 282/2008

    Plasticisers in gaskets(EC) No 372/2007

    as amended

    Ceramics84/500/EEC as amended

    Plastics Elastomersand

    rubbers

    EU legislation

    Active and intelligent materials (EC) No 450/2009

    Regeneratedcellulose film 2007/42/EC

    Food contact materials (EC) No 1935/2004

    Good manufacturing practice (EC) No 2023/2006

    (EU) No 10/2011

      

     

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    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

    contact with food

    • Use of materials for− Food packaging− Kitchen articles− Machines or articles used

    for food manufacture and processing

    NOT

    • Antiques • Covering/coating materials that

    − form part of the food and

    − are consumed with the food

    • Fixed public or private water supply equipment

      

     

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    Slide 11 

     

    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 healthb) bring about an unacceptable change in the composition

    of the foodc) bring about a deterioration in the organoleptic

    characteristics thereof

    Framework Regulation – Article 3

      

     

     

     

    Slide 12 

     

    Framework Regulation – specific measures

    1) Active and intelligent materials and articles

    2) Adhesives

    3) Ceramics

    4) Cork

    5) Rubbers

    6) Glass

    7) Ion-exchange resins

    8) Metals and alloys

    9) Paper and board

    10) Plastics

    11) Printing inks

    12) Regenerated cellulose

    13) Silicones

    14) Textiles

    15) Varnishes and coatings

    16) Waxes

    17) Wood

    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:

      

     

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    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

    EC

    Comitology

    Authorisation

    −+

    Standing Committee on the Food Chain and Animal Health (SCFCAH)

      

     

     

     

    Slide 14 

     

    EU conventions for SML

    • The EU SML are based on toxicology and exposure

    • 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 dm2 of surface • containing the substance at the maximum concentration

    permitted (SML)

    SML (mg/kg food) = NOEL (mg/kg bw) ∙ 60 kg bw / 1 kg food

      

     

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    Slide 15 

     

    • 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

    Framework Regulation – labelling

      

     

     

     

    Slide 16 

     

    • 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

    Framework Regulation – labelling

      

     

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    Slide 17 

     

    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

    Framework Regulation – DoC

      

     

     

     

    Slide 18 

     

    • 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

    Framework Regulation – traceability

      

     

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    Slide 19 

     

    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

    Regulation (EC) No 2023/2006

      

     

     

     

    Slide 20 

     

    • 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

    GMP – minimum requirements

      

     

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    Slide 21 

     

    Questions?

      

     

    Slide 22 

     

    Specific measures

    Plastics

      

     

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    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 

     

    • 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• Coatings

    Regulation (EU) No 10/2011 – scope

    NOT

    • Ion exchange resins• Rubber• Silicones

      

     

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    Slide 25 

     

    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

    Reg. (EC) No 10/2011 – principle of safety

      

     

     

     

    Slide 26 

     

    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 • Polymer production aids

    Substances that may be present in plastic materials:• Non-intentially added substances• Aids to polymerisation

    Reg. (EC) No 10/2011 – principle of safety

    NO

    • Colorants • Solvents

    Subject to national law

    Those not in list

      

     

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     36 

    Slide 27 

     

    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 Mr ≥1000 g/mol for use as additive− Complying requirements regulation− Function as main structural component of final

    material

    Reg. (EC) No 10/2011 – principle of safety

      

     

     

     

    Slide 28 

     

    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

    Reg. (EC) No 10/2011 – Specific migration

      

     

  •  

     37

    Slide 29 

     

    Overall migration = total amount of all non-volatile substances released from a material into food

    • Limit: 10 mg/dm2

    • Infants, young children (0-3) Limit: 60 mg/kg food

    Reg. (EC) No 10/2011 – Principle of inertness

      

     

     

     

    Slide 30 

     

    Layers• not in contact with food and • separated from food by a functional barriermay 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

    Reg. (EC) No 10/2011 – functional barrier

      

     

  •  

     38 

    Slide 31 

     

    Reg. (EC) No 10/2011 – expression of results

    mg/article

    N

    N

    Y

    Y

    Migration test result

    OM?

    Cap, gasket, etc?

    Cap, gasket, etc.?

    Intended use known?

    mg/dm2 total surface article + cap

    Intended use known?

    N

    N N

    N

    N Y

    Y

    mg/kg

    actual content

    Y

    For children?

    Y

    N

    mg/dm2mg/kg

    actual content

    Y

    mg/kg actual content or mg/dm2 total surface article + cap

    V < 0.5L or>10L or S/V inestimable

    For children?

    Y

    mg/kg

    S/V =6

    mg/kg

    actual content

    **

    *

    * DRF may be applicable provided SML ≠ N.D.FRF may be applicable provided SML ≠ N.D and not intended for children (20%

    ** DRF may be applicable

    ******

    For children?

    Y

    N **

    *

    **

    *** DRF may be applicable provided SML ≠ N.D  

     

     

     

     

    Slide 32 

     

    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®

    Reg. (EC) No 10/2011 – new

      

     

  •  

     39

    Slide 33 

     

    • Migration test conditions for storage >30 days @RT10 days @40ºC in Directive 2002/72/EC has been revised:• 10 days @50ºC for storage ≤ 6 months @RT • 10 days @60ºC for storage ≤ 6 months @RTDepending phase transition temperature of polymer• 10 days @40ºC 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

    Reg. (EC) No 10/2011 – new

      

     

     

     

    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 2013 – 31 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. 10/2011

      

     

  •  

     40 

    Slide 35 

     

    • 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: 30 2.5 mg/kg− And others

    Reg. (EC) No 10/2011 – amendments

      

     

     

     

    Slide 36 

     

    • Applicable to polyamide and melamine plastic kitchenware that falls under CN code ex 3924 10 00

    − 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

    Regulation (EU) No 284/2011

      

     

  •  

     41

    Slide 37 

     

    Epoxy derivatives (BADGE, BFDGE, NOGE)• Scope

    − Plastics− Coatings− Adhesives

    • Use and presence of BFDGE, NOGE prohibited• ∑ BADGE, BAGDG∙H2O, BAGDG∙2H2O

    • SML = 9 mg/kg or 9 mg/6 dm2 (V10 l)• ∑ BADGE∙HCl, BAGDG∙2HCl BAGDG∙H2O∙HCl

    • SML = 1 mg/kg or 1 mg/6 dm2 (V10 l)• Appropriate labelling with date of filling

    Regulation (EC) No 1835/2005

    NOT

    • Containers or storage tanks >10 m2

      

     

     

     

    Slide 38 

     

    Questions?

      

     

  •  

     42 

    Slide 39 

     

    Specific measures

    regenerated cellulose

      

     

     

     

    Slide 40 

     

    Regenerated cellulose films

    • Positive lists

    • Restrictions on the substances but not OML

    • Declaration of compliance

    Directive 2007/42/EC

      

     

  •  

     43

    Slide 41 

     

    Specific measures

    ceramics

      

     

     

     

    Slide 42 

     

    Type Type of article Lead Cadmium

    Type 1 Articles not fillable or 0.8 mg/dm² 0.07 mg/dm²H< 25 mm

    Type 2 Articles fillable H>25 mm 4.0 mg/l 0.3 mg/l

    Type 3 Cooking WarePackaging/Vessels V>3L 1.5 mg/l 0.1 mg/l

    Ceramics• Rules for migration testing (4% acetic acid) and analysis• Migration limits for lead and cadmium

    • Compliant if one exeeds >50% of limit, but averageof 3 others are below limit and not exceedding >50% of limit

    • DoC

    Directive 84/500/EEC

      

     

  •  

     44 

    Slide 43 

     

    Specific measures –substances

      

     

     

     

    Slide 44 

     

    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

    Directive 93/11/EEC

      

     

  •  

     45

    Slide 45 

     

    Recycled plastics

      

     

     

     

    Slide 46 

     

    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

    Recycled plastics

      

     

  •  

     46 

    Slide 47 

     

    National Laws

      

     

     

     

    Slide 48 

     

    National rules may derive:

    • 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

    National laws

      

     

  •  

     47

    Slide 49 

     

    FRANCE

    Several décrets,...

    BELGIUM GERMANY NETHERLANDS

    BFR

    ITALY

    Arrêtés royaux 11/5/92 & 3/7/2005

    SPAIN

    Decreto 21/3/1973+Amendments

    RESOLUCION 4/11/1982 warenwet

    •Plastics•Rubbers •RCF••Paper&Paper&PaperboardPaperboard•Glass•Stainless steel

    Macromolec.Compounds

    Lebensm.und Futterm.

    BGBI+

    •53 BFRRecommend.(By Polymer

    Type)+

    Paper & Paper & PaperboardPaperboard

    rec xxxvirec xxxvi

    PlasticsCleaning agents

    CoatingsElastomers&

    rubbersIonisation

    MetalsPaper&Paper&

    PaperboardPaperboardRCF

    Wood

    PlasticsCeramicsCoatings

    ElastomersGlassMetal

    Paper&BoardPaper&BoardRCF

    TextileWood

    PlasticsTin

    RCFPaper &

    PaperboardCeramics

    Glass

    National laws – Member States

      

     

     

     

    Slide 50 

     

    Other EC bodies and European organisationsinvolved in FCM control

      

     

  •  

     48 

    Slide 51 

     

    JRC and EU Reference Laboratory

    Risk management

    (SANCO)

    Official controls

    Member State Authorities and

    Enforcement Laboratories

    As FCM activities 16 years Serving sectorial policies on release of substances from

    food contact materials

    As EU Reference Laboratory

    Methods, migration data, scientific support for FCM

    legislation

    Ad-hoc contributions to EFSA for exposure assessment

    Work

    Supporting Regulation 882/2004 on official food controls Member State

    authorities and enforcement Laboratories (NRLs)

    Work

      

     

     

     

    Slide 52 

     

    • 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

    FVO

      

     

  •  

     49

    Slide 53 

     

    • 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

    FVO

      

     

     

     

    Slide 54 

     

    • 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

    Council of Europe

      

     

  •  

     50 

    Slide 55 

     

    • 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

    Inventory

      

     

     

     

    Slide 56 

     

    • Resolution AP(2004)4: rubber• Resolution AP(2004)5: silicones• Resolution AP(2005)2: packaging inks• Guidelines: glass• Guidelines: paper kitchen towels and

    napkins

    Inventory

      

     

  •  

     51

    Slide 57 

     

    • 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

    Council of Europe

      

     

     

     

    Slide 58 

     

    • 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)

    Inventory lists

      

     

  •  

     52 

    Slide 59 

     

    • 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

    Council of Europe

      

     

     

     

    Slide 60 

     

    • "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

    Council of Europe

      

     

  •  

     53

    Slide 61 

     

    Council of Europe ResolutionsExample – paper and board

      

     

     

     

    Slide 62 

     

    Res. AP (2002)1: General requirements

    Tech Doc No 1: List of substances (incomplete)

    Tech Doc No 2: Guidelines on test conditions and methods of analysis

    Tech Doc No 3: Guidelines for recycled fibres

    Tech Doc No 4: The CEPI Guide for GMP

    Tech Doc No 5: Practical Guide

    Paper and board

      

     

  •  

     54 

    Slide 63 

     

    • Inventory lists• SML and other restrictions are applicable• No OML• GMP• Suitable microbiological quality• No release of substances having an antimicrobial

    effect

    Paper and board

      

     

     

     

    Slide 64 

     

    • 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

    Paper and board

      

     

  •  

     55

    Slide 65 

     

    • CEN standard methodology• Overall migration test methods

    • Analytical methods (standards and technical specification) for testing compliance with SML and QM restrictions

    CEN

      

     

     

     

    Slide 66 

     

    • 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

    RASFF

      

     

  •  

     56 

    Slide 67 

     

    Website on migration testing (JRC)http://ihcp.jrc.ec.europa.eu/our_labs/eurl_food_c_m

    Website on risk assessments (EFSA)http://www.efsa.europa.eu/en/science/afc.html

    Website on legislation (SANCO) http://ec.europa.eu/comm/food/food/chemicalsafety/foodcontact

    /index_en.htm

    Useful links

    Council of Europehttp://www.coe.int/T/E/Social_Cohesion/soc-

    sp/Public_Health/Food_contact/

      

     

     

     

    Slide 68 

     

    New tool: Commission Databasehttps://webgate.ec.europa.eu/sanco_foods/main/?sector=FCM&auth=SANCAS

      

     

  •  

     57

    Slide 69 

     

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

      

     

     

     

     

     

  •  

     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

      

     

  •  

     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

      

     

  •  

     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

      

     

  •  

     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?

      

     

  •  

     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 organolepticcharacteristics thereof

      

     

  •  

     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. 10/2011

      

     

  •  

     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

      

     

     

  •  

     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

    www.jrc.ec.europa.eu

      

     

     

     

    Slide 2 

     

    food contact materials

    smart materials

    intelligent materials

    active materials

    •Monitor the condition of packaged food or the environment surrounding the food

    •Release or absorb substances into or from the packaged food or the environment surrounding the food

    •Extend shelf-life of packaged food

    •Maintain/improve condition of packaged food

      

     

  •  

     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

      

     

  •  

     67

    Slide 5 

     

    Regulation Active and Intelligent materials

      

     

     

     

    Slide 6 

     

    Active materials – absorbers

    • Carbon dioxide

    • Microbial growth

    • Ethene

    • Ripening

    • Oxygen

    • Microbial growth

    • Water

    • Deterioration of food

    • Respiring food + fish/meat

    Food

    Food environment

    Passive layer

    Active layer

    Environment

    packaging

      

     

  •  

     68 

    Slide 7 

     

    Active materials – releasers

    • Carbon dioxide

    • Ethanol

    • Silver

    • Sulphur dioxide

    • grapes

    • Anti-oxidants

    • Flavours

    • Tin

    • simulate canned tomatoes

    • Nitrogen

    • foam on beer Food

    Food environment

    Passive layer

    Active layer

    Environment

    packaging

    anti-microbial

      

     

     

     

    Slide 8 

     

    Smart but not active materials

    Scavengers:

    • Oxygen

    • 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

    Food

    Food environment

    Passive layer

    Active layer

    EnvironmentPET

      

     

  •  

     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 organolepticcharacteristics 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

      

     

  •  

     70 

    Slide 11 

     

    Risk management of substances

    Released active

    substances intended to

    be released

    Substances classified as ‘mutagenic’, ‘carcinogenic’, or

    ‘toxic to reproduction’ Regulation (EC) No 1272/2008

    Substances deliberately

    engineered to nano-particle size

    Authorisation procedure

    Authorisation by relevant Community

    provisions applicable to food

    EU list

    Substances not

    actively released, grafted or behind FB

    Substances used in components

    which are not in direct contact with food and are separated

    from the food by a functional

    barrier

    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

      

    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 

     

  •  

     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 

     

    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

    Non-Community List substances

      

     

  •  

     72 

    Slide 15 

     

    Released?

    Check substance is approved under …

    Flavour Regulation 1334/2008

    Enzyme Regulation 1332/2008

    Y N

    Grafted or immobilised?

    Y

    Y

    N

    N

    N

    Y

    Behind functional barrier?

    Y

    Y

    N

    Specific migration ≤0.01 mg/kg?

    Compliance restrictions in EU list 450/2009?

    N

    N

    Y

    Compliance of substance in component AIM

    Additive Regulation 1333/2008

    Compliant

    Compliance

    Compl. prov. 1935/2004?

    Compl. prov. national leg.?

    Technol. effect on food?

    Y

    No active component

    N

    Not compliant

    CMR or nano?

    NY

    compliance?

    N

    N

    Substance released?

    Y

    Y

      

     

     

     

    Slide 16 

     

    Risk management of anti-microbialsAnti-microbials in food contact materials

    Application

    Max residue limit in food

    Active materialAuthorisation under 528/2012

    Reg. 450/2009

    Authorisation under 1333/2008

    Use

    Food preservativeSurface anti-microbial Process anti-microbial

    Non-mandatory authorisation under 10/2011

    Polymer production aid

    Plastic FCMAuthorisation under national law

    To be clarified yetApplicable 1/9/2013

    5-chlo

    ro-2-m

    ethyl-

    2H-

    isothi

    azol-3

    -one,

    mixtu

    re

    with

    2-meth

    yl-2H

    isothi

    azol-

    3-one

    (3:1)

    in co

    ating

    , pap

    er

    Ag ze

    olite

    A in

    PO, P

    ET, P

    C

      

     

  •  

     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(C8-C22)sulphonic

    acid salts for fresh fish, meat, poultry (EFSA J 2012-10-5-2746)

    − Na carboxymethylcellulose, bentonite, KAl(SO4)2∙12H2O for not direct food contact (EFSA J 2012-10-10-2904)

      

     

  •  

     74 

    Slide 19 

     

    EFSA opinions on active substances

    Oxygen scavengers− Na borohydride, Pd acetate in plastic (EFSA J 2012-10-3-

    2642)− activated carbon, H2O, Fe powder, kaolin calcined, sulphur

    NaCl in sachet (EFSA J 2012-10-3-2643)− (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 2012-10-10-2905)

    − Fe(II) modified bentonite in plastic or sachet (EFSA J 2012-10-10-2906)

      

     

     

     

    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

      

     

  •  

     75

    Slide 21 

     

    Thank you!

    Questions

    http://ihcp.jrc.ec.europa.eu/our_labs/eurl_food_c_m

      

     

     

     

    Slide 22 

     

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

      

     

     

  •  

     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

      

     

  •  

     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

      

     

  •  

     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

      

     

  •  

     79

    Slide 7 

     

      

     

     

     

    Slide 8 

     

    Assignment of simulants vs foods

      

     

  •  

     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°CAny 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.

      

     

  •  

     81

    Slide 11 

     

    Navigating options: OM

    Screening approach

    Solvent extraction #

    Calculate totalmass of extractable

    substances

    Mass < OML?

    Material compliant

    Migration testing

    Choose simulants(s)

    Select exposure Select exposureconditions * conditions *

    Perform migration Perform migration test test

    Migration < OML? Migration test technically feasible?

    Material Material compliant not compliant Migration < OML?

    Perform tests with substitute simulants

    Material Materialcompliant not compliant Migration < OML?

    Material Materialcompliant not compliant

    Yes No

    A, B, C, D1 D2

    Yes No Yes No

    Yes No

    Yes No

    Overall migration

    * 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;  

     

     

     

     

    Slide 12 

     

    OM special cases of simulant assignment

      

     

  •  

     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

      

     

  •  

     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)

      

     

  •  

     84 

    Slide 17 

     

    Navigating options: SM

    Screening approach

    Solvent extraction # Parameters known for migration modelling?

    Determine cP,0 and QM

    Performmodelling

    Calculate migrationassuming 100%

    transferMigration < SML?

    Migration < SML?

    Materialcompliant

    Material compliant

    Migration testing

    Choose simulants(s)

    Select exposure Select exposureconditions * conditions *

    Perform migration Perform migration test test

    Migration < SML? Migration test technically feasible?

    Material Materialcompliant not compliant Migration < SML?

    Perform testswith substitute simulants

    Material Materialcompliant not compliant Migration < SML?

    Material Materialcompliant not compliant

    Yes

    Yes

    Yes

    No

    No

    No

    A, B, C, D1 D2

    Yes No Yes No

    Yes No

    Yes No

    Specific migration –materials not in contact withfoods

    * Exposure conditions may be conventional conditions or accelerated test conditions using defined acceleration factors

    # Theresults 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;

    Not in core text of R10/2011

      

     

     

     

    Slide 18 

     

    Test conditions: time of exposure

      

     

  •  

     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  

     

     

  •  

     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

      

     

  •  

     87

    Slide 23 

     

    Now in practice: OM and SM

      

     

     

     

    Slide 24 

     

    Migration testing

    Single face immersion cell

    Total immersion test

    1 dm2 cutting template

    Pouch testing

    Article filling

    Support for strips

      

     

  •  

     88 

    Slide 25 

     

    Double face testing by immersion

    Single surface testing using

    pouches

    Single surface testing using cells

    article filling

    1 dm2

    equilibrated at Tº

    S1 S2 S3 B1 B2

    + +

    S1 S2 S3 B1 B2

    + simulant at Tº

    filler plug

    clamp screw

    clamp bar

    rubber mat

    food simulant

    lid

    base plate

    sealing ring

    Type A (Pira cell) Type B (TNO cell)

    cell at Tº + liquid at T

    wire gauze support

    simulant

    EXPOSURE (t, T)

    pouch holder at Tº

    hole

    10 x 10 cm

    seal pouch: sides in contact with simulant

    facing

    90 ¼C

    120

    175

    11

    60

    120

    Migration testing

      

     

     

     

    Slide 26 

     

    Testing set-ups for time temperature exposures

    Foods in glass single face cell (e.g. rigid

    films)

    Single cell and simulant

    Total immersion in olive oil

      

     

  •  

     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

      

     

  •  

     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

      

     

  •  

     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 13130 Specific migration plastics• TS 14235 polymeric coatings… and others

    Link CEN: http://www.cen.eu/cenorm/standards_drafts/index.asp

    Other technical specifications• Directives (ceramics, vinyl chloride)• CoE guidelines, national legislations or recommendations

      

     

  •  

     92 

    Slide 33 

     

    CEN methods – overall migrationStandard reference Title Plastics Materials and articles in contact with foodstuffs - Plastics - EN 1186-1:2002 Part 1: Guide to the selection of conditions and test methods for overall migration EN 1186-2:2002 Part 2: Test methods for overall migration into olive oil by total immersion EN 1186-3:2002 Part 3: Test methods for overall migration into aqueous food simulants by total immersion EN 1186-4:2002 Part 4: Test methods for overall migration into olive oil by cell EN 1186-5:2002 Part 5: Test methods for overall migration into aqueous food simulants by cell EN 1186-6:2002 Part 6: Test methods for overall migration into olive oil using a pouch EN 1186-7:2002 Part 7: Test methods for overall migration into aqueous food simulants using a pouch EN 1186-8:2002 Part 8: Test methods for overall migration into olive oil by article filling EN 1186-9:2002 Part 9: Test methods for overall migration into aqueous food simulants by article filling EN 1186-10:2002 Part 10: Test methods for overall migration into olive oil (modified method for use in cases where incomplete extraction of olive oil occurs) EN 1186-11:2002 Part 11: Test methods for overall migration into mixtures of C-labelled synthetic triglycerides EN 1186-12:2002 Part 12: Test methods for overall migration at low temperatures EN 1186-13:2002 Part 13: Test methods for overall migration at high temperatures EN 1186-14:2002 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 EN 1186-15:2002 Part 15: Alternative test methods to migration into fatty food simulants by rapid extraction into iso-octane and/or 95 % ethanol

      

     

     

     

    Slide 34 

     

    5. Slow evaporation of liquid (hot plate)

    4. Removal of specimens, take residual liquid

    1. Glassware weight empty (m1)

    CEN methods – Overall migration aqueous• Exposure to test

    simulant, evaporation to dryness, weight of residue

    L1S1 S2 S3 B1B2

    S1 S2 B1S3 B2mbS1 mbS2 mbS3 mbB1 mbB2

    Overall migration:

    determined by the mass of residue after evaporation of the food simlant

    M = (ma - mb) x 1000

    mg/dm2 S

    S1 S2 B1S3 B2

    2. Sample preparationx 7 samples

    3. Exposure to food simulant (t, T)

    simulant

    S1 S2 S3 B1 B2L06. oven-dessicator to

    weight final mass (m2)S1 S2 B1S3 B2

    mbS1 mbS2 mbS3 mbB1 mbB2

    S1 S2 B1S3 B2

    Valid and reproducible

    results require expertise

      

     

  •  

     93

    Slide 35 

     

    CEN methods –Overall migration oil

    6. GC-FID determination of absorbed oil by FAME -> m3

    3. Remove free oil & weight sample (m2)

    2. Exposure to food simulant (t, T)

    1. Sample weight before exposure (m1)

    5. Derivatisation of absorbed oil byfatty acid methyl esters (FAME)

    4. Extraction of absorbed oil

    (soxhlet)

    simulant

    H20

    H20H20H20

    S1 S2 S3 B2 E1 E2S4 B1

    x 7 samples record masses: ma

    repeat FAME with 6

    standards 0-50 mg oil (C17 spiked) for calibration

    curve

    7. Overall migration:

    Determined by weight loss of specimen

    M = (ma - (mb - mc )) x 1000

    mg/dm2 S

    Valid and reproducible

    results require

    expertise

    E L Bradley, Hong Kong Seminar May 2011

    empty tubes: adjust for loss of volatiles

      

     

     

     

    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

      

     

  •  

     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 13130 for plastics)• EU Reference Laboratory web site:

      

     

  •  

     95

    Slide 39 

     

    SM: plastics (1)

    Standard reference Title

    Plastics Materials and articles in contact with foodstuffs - Plastics substances subject to limitation -

    EN 13130-1:2004 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 13130-2:2004 Part 2: Determination of terephthalic acid in food simulants

    EN 13130-3:2004 Part 3: Determination of acrylonitrile in food and food simulants

    EN 13130-4:2004 Part 4: Determination of 1,3-butadiene in plastics

    EN 13130-5:2004 Part 5: Determination of vinylidene chloride in food simulants

    EN 13130-6:2004 Part 6: Determination of vinylidene chloride in plastics

    EN 13130-7:2004 Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants

    EN 13130-8:2004 Part 8: Determination of isocyanates in plastics

    CEN/TS 13130-9:2005 Part 9: Determination of acetic acid, vinyl ester in food simulants

    CEN/TS 13130-10:2005 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 13130-11:2005 Part 11: Determination of 11-aminoundecanoic acid in food simulants

    CEN/TS 13130-12:2005 Part 12: Determination of 1,3-benzenedimethanamine in food simulants

    CEN/TS 13130-13:2005 Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants

    CEN/TS 13130-14:2005 Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulants

    CEN/TS 13130-15:2005 Part 15: Determination of 1,3-butadiene in food simulants

    CEN/TS 13130-16:2005 Part 16: Determination of caprolactam and caprolactam salt in food simulants

    CEN/TS 13130-17:2005 Part 17: Determination of carbonyl chloride in plastics

    CEN/TS 13130-18:2005 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 13130-19:2005 Part 19: Determination of dimethylaminoethanol in food simulants

      

     

  •  

     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 13130-20:2005 Part 20: Determination of epichlorohydrin in plastics

    CEN/TS 13130-21:2005 Part 21: Determination of ethylenediamine and hexamethylenediamine in food simulants

    CEN/TS 13130-22:2005 Part 22: Determination of ethylene oxide and propylene oxide in plastics

    CEN/TS 13130-23:2005 Part 23: Determination of formaldehyde and hexamethylenetetramine in food simulants

    CEN/TS 13130-24:2005 Part 24: Determination of maleic acid and maleic anhydride in food simulants

    CEN/TS 13130-25:2005 Part 25: Determination of 4-methyl-1-pentene in food simulants

    CEN/TS 13130-26:2005 Part 26: Determination of 1-octene and tetrahydrofuran in food simulants

    CEN/TS 13130-27:2005 Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulants

    CEN/TS 13130-28:2005 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

      

     

  •  

     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

      

     

  •  

     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 simulan