Enlargement and Integration Workshop - JRC …publications.jrc.ec.europa.eu/repository/bitstream...Slide 1 Science for a healthier life Institute for Health and Consumer Protection

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Report EUR 25599EN

Enlargement and Integration Workshop

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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


Slide 14

Packaging

Porous materials:e.g. paper and board

x

z

Food

y

Depiction of chemical migration from a porous material


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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

15

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


NO

• Colorants

• Solvents

Subject to national law

Those not in list

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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


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

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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

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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 (<3 years) and food fat content >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

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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 @RT

Depending 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

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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 (V<500ml v V>10 l)• ∑ BADGE∙HCl, BAGDG∙2HCl BAGDG∙H2O∙HCl

• SML = 1 mg/kg or 1 mg/6 dm2 (V<500ml v V>10 l)• Appropriate labelling with date of filling


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

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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


States

65

Lecture 4: Active and intelligent packaging

Slide 1

Active and intelligent packaging

Eddo J. Hoekstra




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-chloro-2-methyl-2

H-

isothiazol-3-one, m

ixture

with 2-m

ethyl-2Hisothiazol-

3-one (3:1) in

coating, p

aper

Ag zeoliteA in

PO, PET, 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


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 refluxAny 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 B2L0

6. oven-dessicator to weight final mass (m2)

S1 S2 B1S3 B2mbS1 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)



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



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 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

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


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

100

Slide 49


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

101

Slide 51

Exposure time

Slide 52


• Selected exposure conditions = 2 hours at 100°C

102

Slide 53


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


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

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


States

104

Lecture 6: Migration modelling for compliance testing of plastic FCM

Slide 1

Comparison margarine and olive oil vs. modelling

0

500

1000

1500

2000

2500

0 10 20 30

Days

Irgan

ox 1

076

ug/d

m2

MargarineOlive oilmargarine modelolive oil model

Migration modelling for compliance testing of plastic food contact materials

Eddo J. Hoekstra




Slide 2

Compliance test• Verification method • Screening method

Overall migrationResidual contentMigration modellingFood simulant substitutes


4 December 2012 2

FCM not yet in contact Compliant?

no

yesOK

Overestimation of modelled specific migration (section 2.2.3 of Annex I)

Art. 18.3

105

Slide 3

Migration

• Diffusion • Convection • Evaporation• Reaction• Partitioning

4 December 2012 3

tc∂∂

Diffusion is a good simplification for most food contact materials

Slide 4

Monolayer – one dimensional

Fick’s second law of diffusion

4 December 2012 4

2

2

xcD

tc P

PP

∂∂

=∂∂

polymer food (simulant)

F

P

F

PFP c

cK

ρρ

∞

∞=,

,,

At equilibrium (t=∞)

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 constantin place and time

• No migrant in food (simulant) at t=0• The amount of migrant in polymer + food (simulant) is

constant

4 December 2012 5

0,,, PPF mmm =+ ∞∞

Slide 6

• Analytical solution

• Maximum concentration in polymer

Mass transfer equation

4 December 2012 6

⎥⎦

⎤⎢⎣

⎡⎟⎟⎠

⎞⎜⎜⎝

⎛−

+++

Σ−⎟⎠⎞

⎜⎝⎛+

=∞

=t

dDq

qdc

Am

P

Pn

nnPPP

tF2

22210,

, exp1

)1(211 αα

ααα

αρ

∞

∞

∞

∞ ===,

,

,

,

,

1

P

F

P

F

P

F

P

F

P

F

FP mm

VV

cc

VV

K ρρα

nn qq α−=tan

1

22

221exp

1)1(21

1

−∞

= ⎪⎭

⎪⎬⎫

⎪⎩

⎪⎨⎧

⎥⎦

⎤⎢⎣

⎡⎟⎟⎠

⎞⎜⎜⎝

⎛−

+++

Σ−⎟⎠⎞

⎜⎝⎛+

= tdDq

qd

AVSMLMIC

P

Pn

nnPP

FF

αααα

ααρρ

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 algorithmsAnalytical solution serves as reference for validation

4 December 2012 7

Slide 8

Multi-layer – one dimensional

Fick’s second law of diffusion

4 December 2012 8

polymer food(simulant)At equilibrium (t=∞)

n

n

n

n

nnP

P

P

PPP c

cK

ρρ

11

1,

,,

++

+∞

∞=

F

P

F

PFP

nn

n Cc

Kρρ

∞

∞=,

,,

2,

2

,22,

2

2,21,

2

1, ...xc

Dxc

Dxc

Dt

c nPnP

PP

PP

P

∂∂

++∂∂

+∂∂

=∂∂

19

108

Slide 9

⎟⎠⎞

⎜⎝⎛ −+−=

RTRMMAD rrPP

10454003.01351.0exp 3/2**

Estimation of diffusion coefficient

Different approaches• Arrhenius

• Estimation (Piringer)

4 December 2012 9

⎟⎠⎞

⎜⎝⎛ −=

RTEDD A

P exp0

(m s−2)

Polymer specific constant

Polymer specific temperature constantTAA PP

τ−= '**

Reference activation energy

Slide 10

Estimation of AP’ for each T

4 December 2012 10

R. Brandsch, 2010

109

Slide 11

Estimation of Ap’*

4 December 2012 11

R. Brandsch, 2010

Slide 12

Applicability for polyolefins

cP,0 < 1%KP,F = 1 for high solubility of migrant in food.KP,F = 1000 for low solubility of migrant in food.

4 December 2012 12

11.5

13.1

14.5

11.5

AP'*

0

1577

1577

0

τ (K)

PP (rubber)

PP (random)

PP (homo)

HDPE

LLDPE

LDPE

Polymer

<100

<120

<120

<90

<100

<80

T (°C)

30 - 2000

30 - 2000

30 - 2000

30 - 2000

30 - 2000

30 - 2000

Mr (Da)

110

Slide 13

Polymer specific constant

High AP

4 December 2012 13

High DP

More flexible polymer

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 2012 14

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 2012 15

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 foodmaximum temperaturemaximum packaging timeIntended highest surface-to-volume ratio

4 December 2012 16

112

Slide 17

References (http://ihcp.jrc.ec.europa.eu/our_labs/eurl_food_c_m)

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 24514 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 (Ap’*) and

polymer specific “activation temperature” constant (t) for mathematical modelling

of a plastic food contact materials. In preparation4 December 2012 17

Slide 18


113

Lecture 7: Correction factors of experimentally determined specific migration

Slide 1

Correction factors of the experimentally determined specific migration

Eddo J. Hoekstra




Slide 2

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 lipophilicsubstances migrating into food with a fat content of more than 20% (Section 4.1 of Annex V)


2. correction for the simulant D2 Reduction Factor (DRF) for defined foods (Section 4.2 of Annex V)


3 correction factors for specific migration

4 December 2012 2

Fat consumption is maximum 200 g

D2 greater extraction capacity compared to food

114

Slide 3

Formula

• Surface-to-volume ration difference

• DRF = 1-5 (see Table 2 Annex III)

• FRF

c = concentration fat in food (g fat/kg food)cmax = maximum fat intake per day = 200 g fat/kg foodc% = percentage of fat in food (% fat) > 20%FRF = 1-5

• TRF = DRF ∙ FRF ≤ 5

4 December 2012 3

(mg/kg)

VS

VS

M M

test

realtestS/V

⎟⎠⎞

⎜⎝⎛

⎟⎠⎞

⎜⎝⎛

=

1005 c

cc FRF %max

==

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 2012 4

115

Slide 5

5

Compliance of experimental specific migration (Mtest)

Contact with food for infants/young children?

S/V is impractical to estimate

Y

N

N

Y

Y

Listed “yes” in column 7 of Table 1 of Annex I?

Y

N

(S/V)test = (S/V)real?(dm²/kg)

Y

N

Food simulant A, B, C, D1, E?

Y

N

N

MS/V = MtestMS/V = Mtest (S/V)real/(S/V)test (mg/kg)

food with ≤ 20% fat?

1

2

Slide 6

6

Test with food?

Y

N

MDRF≤SML

MS/V≤SML ≤ 60 mg/kg

Non-compliant

N

NN

Compliant

Y

Y

Y

Select DRF

N

Y

M≤SML

V<0.5 l v V>10 l v films

M=MS/V*6/(S/V)real

M≤SML ≤60 mg/kg

N

Y

N Y

Food simulant D2?

Y

N

MDRF = MS/V

Y

N

Child food?N

Y

MDRF = MS/V/DRF

M=MDRF*6/(S/V)real


SML=ND?

N

Y

Child food?

Y

1

116

Slide 7

7

2

N Y

TRF=FRF*DRF

TRF>5

TRF=5

Y

MTRF=MS/V/TRF

N

MTRF≤SMLN

Y

MFRF=MS/V/FRF

MFRF≤SML

Non-compliant

Compliant

M=MS/V*6/(S/V)real

M≤SML≤60 mg/kg

Y

Y

N

Y

MS/V≤60 mg/kg

Y

NY

N V<0.5 l v V>10 l v films

Y

NN

Calculate FRF= g fat/kg food /200= % fat *5/100

Select DRF


Calculate FRF= g fat/kg food /200= % fat *5/100

M=MTRF*6/(S/V)real

M≤SML

Test with food?

N

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 25112 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 2012 8

117

Slide 9


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

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 evaluationsClearances in other jurisdictions (e.g., U.S. FDA)CoE Resolutions

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: General requirementsTech 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 fibresTech Doc No 4: The CEPI Guide for GMPTech Doc No 5: Practical Guide

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

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 DocumentDeveloped by CEFIC, CEPI, CITPA, FPE

http://www.eurosac.org/eurosac/pdf/11796_Industry-Guideline-Food-Contact-%28CEPI-and-CI.pdf

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 15519 Preparation of an organic solvent extract

EN 14338 Conditions for determination of migration from paper and board using modified polyphenylene oxide (MPPO) as simulant

124

Slide 13

Paper and board – methods

EN 12498 Determination of cadmium, lead and chromium in an aqueous extract

EN 12497 Determination of mercury in an aqueous extract

EN ISO 15320 Determination of pentachlorophenol in an aqueous extract

EN 1104 Determination of transfer of antimicrobic constituents

Slide 14


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

125

Slide 15


CEN/TS 13130-13 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

126

Slide 17

Migration into Tenax

EN 14338 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

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

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 factorsProposal by the paper and board industry

129

Slide 23

yOther (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 12983-2:2005

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 8442-1:1997 Part 1: Requirements for cutlery for the preparation of food EN ISO 8442-2:1997 Part 2: Requirements for gold-plated cutlery EN ISO 8442-2:1997 Part 2: Requirements for stainless steel and silver-plated cutlery EN ISO 8442-3:1997 Part 3: Requirements for silver-plated table and decorative holloware EN ISO 8442-4:1997 Part 4: Requirements for gold-plated cutlery EN ISO 8442-5:2004 Part 5: Specification for sharpness and edge retention test of cutlery EN ISO 8442-6:2000 Part 6: Lightly silver plated table holloware protected by lacquer EN ISO 8442-7:2000 Part 7: Specification for table cutlery made of silver, other precious metals and their alloys EN ISO 8442-8:2000 Part 8: Specification for silver table and decorative holloware

Standard methods

Slide 24

Standard methods


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 6486-1:1999 Ware: Release of lead and cadmium — Part 1: Test method

ISO 6486-2: 1999 Ware: Release of lead and cadmium -- Part 2: Permissible limits

ISO 8391-1: 2002 Cookware: Release of lead and cadmium -- Part 1: Method of test

ISO 8391-2 : 2002 Cookware: Release of lead and cadmium -- Part 2: Permissible limits

Cook and tableware Materials and articles in contact with foodstuffs - Silicate surfaces -

EN 1388-1:1995 Part 1: Determination of the release of lead and cadmium from ceramic ware

EN 1388-2:1995 Part 2: Determination of the release of lead and cadmium from silicate surfaces other than ceramic

ware

130

Slide 25

Standard methods


Glass Glass hollowware in contact with food

ISO 7086-1: 2005, Release of lead and cadmium -- Part 1: Test method

ISO 7086-2: 2005, Release of lead and cadmium -- Part 2: Permissible limits

Enamel Vitreous and porcelain enamels

ISO 4531-1, 2003, Release of lead and cadmium from enamelled ware in contact with food -- Part 1: Method of test

ISO 4531-2, 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

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

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

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

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

135

Slide 35

GC-MSFull scan EI mass spectrum

40 60 80 1001201401601802002202402602803003203403603804004204400

5000

10000

15000

20000

25000

30000

35000

40000

45000

50000

55000

60000

65000

70000

75000

80000

85000

90000

m/z-->

Abundance

Average of 27.747 to 27.818 min.: (-)383

208

149

297104

235 35776 33926456

183429401125

314 449

Typical of a PET oligomer

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

136

Slide 37

LC-TOF-MS analysis Mass accurate to within 3 ppm

Software predicts molecular formula

Working with industry each potential migrant

can be identified

TIC

m/z, amu0.00

2.50

5.00

7.50

10.0Intensity x 104, counts

[M+NH4]+444.1648

[M+Na]+449.1203

[M+K]+465.0897[M+H]+

427.1346

17 amu 5 amu 16 amu

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

137

Slide 39

Printing inks

Commission Regulation (EC) No 2023/2006 on GMP, Annex I specifically deals with printing inks

Swiss Ordinance

German recommendations

Photoinitiatorse.g. benzophenone, ITX

Set-off

Slide 40

• Rubber

• Silicones

• Cork

• Ion exchange resins

• Colourants

• Polymerisation aids

• Crystal glass

Council of Europe Resolutions

Other

138

Slide 41

Cookware and tableware

Coatings on metal substrates• Same approaches as coatings applied to cans• Perfluoro- compounds

Metals and alloysCouncil 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

139

Slide 43

http://www.coe.int/t/e/social_cohesion/soc-sp/public_health/Food_contact/

Slide 44

http://www.coe.int/t/e/social_cohesion/soc-sp/public_health/Food_contact/

140

Slide 45


States

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

2

TENAX®

- registered trademark for poly(2,6-diphenyl-p-phenylene oxide)(MPPO – Tenax® TA);

- particle size 60-80 mesh;

- pore size 200 nm;

- high molecular weight, 500 000 to 1 000 000 dalton;

- very high temperature stability Tmax = 350°C;

- high surface area and low specific mass, 0.25 g/cm3;

- 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

143

Slide 5

www. sisweb.com

Tenax® TA

Slide 6

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

7

TENAX® in Regulation (EU) No 10/2011

Annex III2. 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

Slide 8

8



Ref. no. Description of food Food simulants – E

02

02.01

02.02

02.03

02.04

02.05

02.06

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:


B. Other

X

X

X

X

X

X

145

Slide 9

9



03

03.02

03.03

04

04.02

04.03

Chocolate, sugar and products thereof

Confectionery products

A. In solid form:

I. With fatty substances on the surface

II. Other

Sugar and sugar products

A. In solid form: crystal or powder

Fruit, vegetables and producs thereof

Processed fruit:

A. Dried or dehydrated fruits, whole, sliced, flour or powder

Nuts (peanuts, chestnuts, almonds, hazelnuts,, walnuts, pine kernels and

others):

A. Shelled, dried, flaked or powdered

B. Shelled and roasted

X

X

X

X

X

Slide 10



04.05

06

06.05

07

07.01

07.04

08

08.03

Processed vegetables:

A. Dried or dehydrated vegetables whole, sliced or in thhe form of flour or

powder

Animal products and eggs

Whole eggs, egg yolk, egg white

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

X

X

146

Slide 11

11



08.06

08.08

08.09

08.12

08.13

08.14

Sandwiches, toasted bread pizza and the like containing and kind of

foodstuff


B. Other

Dried foods:


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

X

Slide 12

12


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

13

CEN methods

Slide 14

14

EN 1186-13; 2002Materials and articles in contact with foodstuffs

– PlasticsPart 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

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 6hwith diethyl ether;

- Spread the MPPO in a Petri dish of a suitable diameter and placethe dish in a fumehude;

- Allow the ether to evaporate while frequently mixing witha glass rod;

- Place the dish in an oven at 160°C for 6h;

- After heating store the MPPO in closed conical flask.

Slide 16

16

Cleaning procedure - Notes

Note1. Heating of MPPO saturated with diethyl ether can be explosive.Therefore, it should be ensured that diethyl ether is completelyevaporated 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

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 dm2 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. Thereforeit can be necessary to include a procedure to control of the timeand temperature in order to achieve reproducible and repeatableresults;

Slide 18

18

Exposure to MPPO:

Note 2. In the case of the articles of irregular geometry and with notflat areas. Possible solutions are to cut the appropriate parts andmix with MPPO using the conventional mass of MPPO (4 g/dm2)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 downto room temperature without removing the glass covers (takes approximately 0.5h).

150

Slide 19

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 etherneeded for extraction

Mass of the MPPO Volume of

diethylether for 1st

extraction

Volume of

diethylether for 2nd

extraction

Volume of

diethylether for 3rd

extraction

1 20 30 30

2 30 30 30

5 50 30 30

10 90 40 40

Slide 20

20


- Pour the diethyl ether through the funnel into the Erlenmeyer flaskand shake manually 1 min.,

- Allow the Erlenmeyer flask and its content to stand for 1 min, withoutshaking;

- 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;

- Rinse the filter with 10 ml diethyl ether;

- Concentrate the combine diethyl ether solutions to approximately 5ml, first using rotary vapour then gently nitrogen flow;

151

Slide 21

21


- Weigh the 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;

- Evaporate the 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 ofthe vial from the stable mass of the vial and residue;

Slide 22

22

Expression of results:

M=(ma-mb)/s

M – is the mass of the migrated substances adsorbed onto MPPO from the test specimen, in milligrams per square decimeter;

ma – is the mass of the residue from the MPPO that had been in contactwith the test specimen;

mb – 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

23

DIN EN 14338; 2004Paper 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;

Slide 24

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 withacetone;

- 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

25

Cleaning procedure - Notes

Note 1. MPPO can be used repeatedly if cleaned in this way betweenuses;

Note 2. When drying MPPO in a forced air oven the dishes should be covered to prevent the MPPO from blowing about

Slide 26

26

Exposure to MPPO (duplicate):

- to cover the food contact surface sufficiently, 4 g MPPO per 1dm2 of surface area of the test specimen is required;

Note 1.Cell according to EN 1186-13 or Petri dish without the glass ring

Note 2. Bed of MPPO should cover all test specimen, to uniform depthwhen the test sample is placed into the oven

Paper

154

Slide 27

27

Exposure to MPPO:

Note 3. Petri dish should be placed into preheated incubator and startthe time when the temperature has recovered to a temperaturewithin 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 downto room temperature without removing the glass covers (takes approximately 0.5h).

Slide 28

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 ILC02 2011

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

30

Cleaning procedure – according to DIN EN 14338 – 6h soxhletextraction 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 dm2

of surface area; higher amount of Tenax® were used to ensure complete contact between the test specimen and Tenax® ;

156

Slide 31

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 insidethe 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 foilsurface covered by Tenax®;

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 flaskusing funnel.

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 spikingas a blank.

Slide 34

Extraction of the Tenax®:

- Transfer 1.0 g of the Tenax® (or all the Tenax® from the Petri dishafter migration) into the 40 mL vial;

- Add 20 mL of extraction solution (Hexane + 2.5 ppm of BBP);

- Shake manually for 1 min;

- Leave it for 5 min without shaking;

- Insert the funnel with the filterinto a new 40mL vial;

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 inthe 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.

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 !

38

160

Slide 39


States

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

162

Slide 3

Official controls

Guarantee the safety of foods and ensure their free circulation in the EU

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 assessment =exposure assessment + hazard characterisation

Risk management (RM)=accounting and addressing

(SANCO)

Official controls =

RASFF + implementation/

enforcement of RM

Consumer protection and trust

EU-RL - NRLs

Communication =transparency

interactive process

(toxicology)

Slide 4

http://crl-fcm.jrc.ec.europa.eu/files/Method_Perf_Guidelines_final_ed2009.pdf

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

163

Slide 5

Quality assurance QA)

Quality assurance with accreditation ISO 17025

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 17025 Accreditation based QA

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 17025• If conform to ISO 17025 the assessing body attests conformity

through a certificate• Accreditation is tested every year

EU-RL and NRLs: MUST be accredited 17025 in 882/2004 OFFC

Slide 8

Accreditation

Accreditation bodies around the world

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 qualityCan always prove laboratory quality

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)

167

Slide 13

How can these controls be achieved nin 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 nin practice?3rd line possibilities• Participation in Proficiency testing (PT) scheme

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

169

Slide 17

Characterisation of methods of analysis

RecoverySelectivitySensitivityLinearityMeasurement uncertaintyOther criteria that may be selected as required

Accuracy;Applicability• matrix and concentration rangeLimit of detectionLimit of determination / quantificationPrecisionRepeatabilityReproducibility

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….

170

Slide 19

Precision parametersRelationship between R, RL and r

labslab

run

Repeatability, r

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 5725

171

Slide 21

Measurement Uncertainty

Parameter charactering the dispersion of the values of results of a measurement.

Different approaches • AOAC • EURACHEM http://www.measurementuncertainty.org/

.

Random errors (sdev) Systematic errors (bias) -0,20

-0,15

-0,10

-0,05

0,00

0,05

0,10

0,15

0,20

-0,20 -0,15 -0,10 -0,05 0,00 0,05 0,10 0,15 0,20

s

δ

-0,20

-0,15

-0,10

-0,05

0,00

0,05

0,10

0,15

0,20

-0,20 -0,15 -0,10 -0,05 0,00 0,05 0,10 0,15 0,20

s

-0,20

-0,15

-0,10

-0,05

0,00

0,05

0,10

0,15

0,20

-0,20 -0,15 -0,10 -0,05 0,00 0,05 0,10 0,15 0,20

s

-0,20

-0,15

-0,10

-0,05

0,00

0,05

0,10

0,15

0,20

-0,20 -0,15 -0,10 -0,05 0,00 0,05 0,10 0,15 0,20

δ

Slide 22

Importance of method performance and criteria in compliance assessment

Eurachem/CITAC Guide, 2007

Non-compliantCompliant

Slide 23

172

Use of Measurement Uncertainty (MU) in compliance assessmentRules 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 25

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 17025 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

174

Slide 27

PT- a duty for official controls

A control laboratory has requirements to be accredited e.g17025

• Accreditation checks the process

A control laboratory should also use PTs as self check on performance vs. others

9 55 74 45 59 12 36 77 79 6 64 30 16 40 54 62 84 48 15 29 58 23 8 50 17 81 46 1 75 65 3 63 72 18 27 35 57 53 39 51 19 4 69 25 71 66 76 52 21 83 38 67 7 43 68 70 5 26 61 20 34 44 33 11 24 78 49 60 47 2 14 42 82 32 13 10 22 73 28 37 31

2.7

4.9

7.1

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

6.0

Laboratory Number

z-score

Slide 28

Organisation of proficiency testing (PT)

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)VWAKIWATNORIKILTLGC

• More info: EPTIS database lists PT schemes (PTS) operated in Europe, the Americas and in Australia. The focus is on the field of testing;http://www.eptis.bam.de

EU-RL organised inter-laboratory trials

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 2011 – 2012

Series 11 OM into an aquous simulantOM into olive oil

Series 12Phthalates in simulantMelamine in simulantPAAs in simulantBisphenol A in simulantPhotonitiators

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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

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


States

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 2012. 14 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 emails “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 67/11/2012 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

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.

181

Annex 1 - Highlights photos from the training

182

Annex 2 - Participants

NP: did not participate

183

Annex 3 - Customer satisfaction survey

184

Customer satisfaction survey results

Programme

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Objectives

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Contents, quality of presentations

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Discussion time / interaction between participants

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Workshops / sub‐sessions

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Balance between sessions

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

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Supporting material

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Provision of additional resources (useful links, downloads, contacts)

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Organisation

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Location

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Side events (lunch, coffee break)

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Online registration

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

Overall evaluation of the event

Very good

Good

Satisfactory

Could be improved

Unsatisfactory

N/A

No answer

185

European Commission EUR 25599 – 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 2012 – 181 pp. – 21.0 x 29.7 cm EUR – Scientific and Technical Research series –ISSN 1831-9424 (online) ISBN 978-92-79-27392-6 (pdf) doi:10.2788/67212 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 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 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.

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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.

LB-N

A-25599-EN

-N

Documents

Enlargement and Integration Workshop - JRC …publications.jrc.ec.europa.eu/repository/bitstream...Slide 1 Science for a healthier life Institute for Health and Consumer Protection