Upload
others
View
14
Download
0
Embed Size (px)
Citation preview
1
Report EUR 25599EN
Enlargement and Integration Workshop
2 0 1 2
C. Simoneau, E. Hoekstra, N. Jakubowska
“EU legislation and testing for the chemical testing of food contact materials” Ispra, 6-7 November 2012
2
European Commission Joint Research Centre Institute for Health and Consumer Protection Contact information Catherine Simoneau Address: Joint Research Centre, Via Enrico Fermi 2749, TP 260, 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
3
Executive Summary
In the framework of the "Enlargement and Integration initiative", the European Commission Joint Research Centre (JRC) organised a training workshop focusing the latest EU Directives and legislative requirements for food contact materials (FCM), and details of the experimental procedures for compliance testing against the requirements. The training was conceived by the operating manager of the EURL‐FCM C. Simoneau. The programme included lectures and test demonstrations by C, Simoneau, E. Hoekstra, and N. Jakubowska. The workshop took place in Ispra on 6‐7 November 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.
4
Table of contents
Executive Summary...................................................................................................................................3 Table of contents ........................................................................................................................................4 Programme....................................................................................................................................................5 Presentations ...............................................................................................................................................6 Lecture 1: Introduction to food contact materials ..................................................................6 Lecture 2: EU Directives and legislative requirements for FCM............................. 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
5
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)
6
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
7
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
8
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)
9
Slide 7
Importance of packaging
Packaging is beneficial
• Protects foodstuff from spoilage
However the transfer of chemicals from packaging to food may have a negative impact on the quality and safety of the food
• No food contact material is completely inert
• Need to ensure the safety of these materials
Slide 8
Contamination from food packaging
Prolonged contact between food and non-food material
Possibility that ingredients from the packaging could be transferred into the food = migration
10
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
11
Slide 11
Factors affecting migration
Migration is a diffusion and partitioning process that is dependent on:
• The nature of the food contact material (FCM)• The nature and concentration of the migrating substance• The nature of the foodstuff• The nature, the extent and the type of contact between the food
contact material/article and the foodstuff
Slide 12
Packaging
Impermeable materials:- glass & ceramics- metals & alloys
xyz
Food
Depiction of chemical migration from an impermeable material
The nature of the FCM
12
Slide 13
Packaging
Permeable materials: - plastics- rubber & silicone- coatings
xy
z
Food
Depiction of chemical migration from a permeable material
The nature of the FCM
Slide 14
Packaging
Porous materials:e.g. paper and board
x
z
Food
y
Depiction of chemical migration from a porous material
The nature of the FCM
13
Slide 15
The nature of the substance
Ingredients needed to make plastics• Monomers and starting substances• Catalysts• Solvents and suspension media• Additives
Antioxidants, antistatics, antifogging, slip additives, plasticisers, heat stabilisers, nucleating agents, dyes and pigments
Slide 16
M.P Steven, Journal of Chemical Education, 1993, 444
Typical additives for plastics
StabilisersUV absorbersPreservativesOptical brightenersFoaming agentsRelease agentsetc
Anti-oxidantsPlasticisersLubricantsEmulsifiersFillersFlame retardantsImpact modifiers
14
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
16
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
17
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
18
Slide 25
Potential migrants from recycled FCMs
• Incomplete cleaning of substrate
• Mis-use of FCMs entering into the recycled food packaging stream• e.g. detergents, industrial chemicals
• Non-FCM materials and articles entering into the recycled food packaging stream• e.g. newspaper and magazine print
Slide 26
Safety of food contact materials
• Prevent migration of chemicals to food in unsafe levels
• Allow use of substances (toxicological data)• Impose limits of migration
• Overall migration + Specific migration for each substance
• Testing: need of (harmonised) methods
• Number of substances (> 3000) and materials • Testing = migration & (identification – quantification)
19
Slide 27
Food contact safety: who does what?
Risk assessment: • European Food Safety Authority (EFSA)
Risk management: • Commission DG Health and Consumer Protection (SANCO),
Enforcement: • Member States
Slide 28
Food contact safety: who does what?
Monitoring and inspection: • National Official Control Laboratories supported by National
Reference Laboratories
Scientific support: • European Union Reference Laboratory (JRC) • Regulation OFFC EC/882/2004 supported by Network of NRLs
20
Slide 29
Remarks
Consumers demand • High food quality maintained by packaging (active too) • Convenience by packaging (resealable, monoportions etc)• Food protection by packaging (product integrity)
Packaging technology must respond to needs• Barrier to bioterrorism (integrity, intelligent)• Waste reduction: 3Rs (recyclability, biobased)• Information carrier (labelling); traceability
Slide 30
Remarks
Packaging technology must also:• Not be a source of contamination to the food
Role of legislation, risk assessment and monitoring enforcement:
• The inspections are crucial • The laboratories are crucial
21
Slide 31
Seminar programme
1. EU Directives and legislative requirements for FCM;
2. Framework of implementation of the EU legislation on FCM;
3. Active and intelligent materials
4. Compliance testing for plastics overall and specific migrations )
Slide 32
Seminar programme
5. Method validation and verification for testing procedures for compliance testing;
7. Reference materials and proficiency testing programmes;
8. Kitchenware and worked examples
22
Slide 33
The content of this lecture does not necessarily represent the position of the European Commission or the EU Member
States
23
Lecture 2: EU Directives and legislative requirements for FCM
Slide 1
EU Directives and legislative requirements for food contact materials
Eddo J. Hoekstra
Joint Research Centre
The European Commission’s in-house science service
www.jrc.ec.europa.eu
Slide 2
EU legislationon food contactmaterials
24
Slide 3
Overview
• Introduction and general principles • EC legislation of Food Contact Materials (FCMs)• Other legal or recommended provisions in the EU• Framework of implementation of EU legislation on FCM
Slide 4
Who does what
• Risk management− European Commission (DG SANCO)
• Risk assessment + sampling advice− European Food Safety Authority (EFSA)
• Official control− MS competent authorities
• High quality and uniformity of analytical results− European Union Reference Laboratory for FCM (EU-RL)− Food and Veterinarian Office (FVO)
• Other European organisations− Council of Europe (CoE)− European Standardisation Organisation (CEN)
25
Slide 5
European Union
Croatia
Slide 6
How and when did it all start?
Vinyl chloride monomer (VCM)1972 – cause of liver cancer in laboratory 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)
26
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
27
Slide 9
Framework Regulation (EC) No 1935/2004
Food contact materials• First step to harmonising legislation• Defines what is meant by ‘food contact materials and
articles’• Two general principles− Inertness− Safety
Slide 10
Framework Regulation – scope
• Materials and articles − in contact with food− intended for food contact− expected to come into
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
28
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:
29
Slide 13
Framework Regulation – role of EFSA
• Any provision which may affect public health shall be adopted after consulting the European Food Safety Authority (EFSA)
• When there is a positive list any substances included in this list should first be evaluated by EFSA
• Procedure:
manufacturer MS competent authority EFSA
Other MS CA
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
30
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
31
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
32
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
33
Slide 21
Questions?
Slide 22
Specific measures
Plastics
34
Slide 23
Plastics
First material type to be covered by specific measures• Directive 82/711/EEC basic rules for testing migration• Directive 85/572/EEC list of simulants to be used for
testing migration• Directive 90/128/EEC• Directive 2002/72/EC• Regulation (EU) No. 10/2011
Slide 24
• 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
35
Slide 25
Specific authorisation of substances• Suitable technical quality and purity of substance• Restrictions− Specific migration limit (SML)−Maximum permitted quantity in the material (QM)− Overall migration limit (OML)− Other restrictions and specifications
• Substances in nanoform shall only be used if explicitly authorised
Reg. (EC) No 10/2011 – principle of safety
Slide 26
List of substances authorised for use in plastic food contact materials and articles shall contain:
• Monomers and other starting materials• Macromolecules from microbial fermentation • Additives • Polymer production aids
Substances that may be present in plastic materials:• Non-intentially added substances• Aids to polymerisation
Reg. (EC) No 10/2011 – principle of safety
NO
• Colorants • Solvents
Subject to national law
Those not in list
36
Slide 27
Substances not listed but authorised for use in plastic food contact materials and articles
• Salts of authorised acids, phenols, alcohols with Al, Ba, Ca, Co, Cu, Fe, K, Li, Mg, Na, Zn
• Mixtures of authorised substances without chemical reaction
• Pre-polymers and natural and synthetic macromolecules of authorised monomers or starting substances: for use as monomers or starting substances
• natural and synthetic polymeric substances with Mr ≥1000 g/mol for use as additive− Complying requirements regulation− Function as main structural component of final
material
Reg. (EC) No 10/2011 – principle of safety
Slide 28
Specific migration = the amount of a substance released from a material into food
• Limit expressed in mg/kg• No limit SML = 60 mg/kg• Additives also authorised as food additives or
flavourings− In authorised foods: shall not exceed
restrictions/SML in Reg. (EC) No 1333/2008, Reg. (EC) No 1334/2008 or this Reg. Annex I
− In non-authorised foods: shall not exceed restrictions/SML in this Reg. Annex I
Reg. (EC) No 10/2011 – Specific migration
37
Slide 29
Overall migration = total amount of all non-volatile substances released from a material into food
• Limit: 10 mg/dm2
• Infants, young children (0-3) Limit: 60 mg/kg food
Reg. (EC) No 10/2011 – Principle of inertness
Slide 30
Layers• not in contact with food and • separated from food by a functional barriermay be manufactured with substances not listed, but not:• mutagenic, carcinogenic, toxic to reproduction• in nanoform
• Specific migration not detectable with statistical certainty and a LoD of 0.01 mg/kg
• LoD shall also apply to a group of substances that are structurally and toxicologically related
• Limit includes set-off transfer
Reg. (EC) No 10/2011 – functional barrier
38
Slide 31
Reg. (EC) No 10/2011 – expression of results
mg/article
N
N
Y
Y
Migration test result
OM?
Cap, gasket, etc?
Cap, gasket, etc.?
Intended use known?
mg/dm2 total surface article + cap
Intended use known?
N
N N
N
N Y
Y
mg/kg
actual content
Y
For children?
Y
N
mg/dm2mg/kg
actual content
Y
mg/kg actual content or mg/dm2 total surface article + cap
V < 0.5L or>10L or S/V inestimable
For children?
Y
mg/kg
S/V =6
mg/kg
actual content
**
*
* DRF may be applicable provided SML ≠ N.D.FRF may be applicable provided SML ≠ N.D and not intended for children (20%
** DRF may be applicable
******
For children?
Y
N **
*
**
*** DRF may be applicable provided SML ≠ N.D
Slide 32
Revised list of food simulants• non-acidic, non-alcoholic, non-fatty foods – simulant is
10% ethanol• alcoholic foods containing up to 20% alcohol – simulant is
20% ethanol• dairy, cloudy, and high-alcohol beverages – simulant is
50% ethanol• fatty foods – simulant is vegetable oil (meeting certain
specifications)• acidic food – simulant is 3% acetic acid• dry foods – simulant is poly(2,6-diphenyl-p-phenylene
oxide), commonly known as Tenax TA®
Reg. (EC) No 10/2011 – new
39
Slide 33
• Migration test conditions for storage >30 days @RT10 days @40ºC in Directive 2002/72/EC has been revised:• 10 days @50ºC for storage ≤ 6 months @RT • 10 days @60ºC for storage ≤ 6 months @RTDepending phase transition temperature of polymer• 10 days @40ºC scientific evidence that migration has
reached equilibrium under this test condition
• Separate test conditions for verifying compliance with OML and SML− OML: fewer combinations of contact time and
temperature
Reg. (EC) No 10/2011 – new
Slide 34
Implementation of technical changes
• Until 31 December 2012, compliance documents should be based on migration testing using:− food simulants specified in 85/572/EEC and − test conditions specified in 82/711/EEC
• From 1 January 2013 – 31 December 2015, compliance documents should be based on migration testing using: − food simulants specified in the (EC) No. 10/2011 and − test conditions specified in 82/711/EEC or− test conditions established in the (EC) No. 10/2011
• From 1 January 2016, compliance documents should be based on migration testing using: • food simulants + test conditions specified in (EC) No. 10/2011
40
Slide 35
• Regulation (EU) No 321/2011− bans the use of Bisphenol A (BPA) for the manufacture
of polycarbonate infant feeding bottles• Regulation (EU) No 1282/2011− Melamine SML: 30 2.5 mg/kg− And others
Reg. (EC) No 10/2011 – amendments
Slide 36
• Applicable to polyamide and melamine plastic kitchenware that falls under CN code ex 3924 10 00
− Primary aromatic amine release from polyamide kitchenware
− Formaldehyde release from melamine-ware
• Products originating in or consigned from China and Hong Kong are controlled
• Prior Notification by importer is required to notify competent authority of the estimated date and time of physical arrival of the consignment 2 working days in advance
• Documentary checks on 100% of consignments
• Identity and physical checks on 10% of consignments
− Random selection
− including laboratory testing
Regulation (EU) No 284/2011
41
Slide 37
Epoxy derivatives (BADGE, BFDGE, NOGE)• Scope
− Plastics− Coatings− Adhesives
• Use and presence of BFDGE, NOGE prohibited• ∑ BADGE, BAGDG∙H2O, BAGDG∙2H2O
• SML = 9 mg/kg or 9 mg/6 dm2 (V10 l)• ∑ BADGE∙HCl, BAGDG∙2HCl BAGDG∙H2O∙HCl
• SML = 1 mg/kg or 1 mg/6 dm2 (V10 l)• Appropriate labelling with date of filling
Regulation (EC) No 1835/2005
NOT
• Containers or storage tanks >10 m2
Slide 38
Questions?
42
Slide 39
Specific measures
regenerated cellulose
Slide 40
Regenerated cellulose films
• Positive lists
• Restrictions on the substances but not OML
• Declaration of compliance
Directive 2007/42/EC
43
Slide 41
Specific measures
ceramics
Slide 42
Type Type of article Lead Cadmium
Type 1 Articles not fillable or 0.8 mg/dm² 0.07 mg/dm²H< 25 mm
Type 2 Articles fillable H>25 mm 4.0 mg/l 0.3 mg/l
Type 3 Cooking WarePackaging/Vessels V>3L 1.5 mg/l 0.1 mg/l
Ceramics• Rules for migration testing (4% acetic acid) and analysis• Migration limits for lead and cadmium
• Compliant if one exeeds >50% of limit, but averageof 3 others are below limit and not exceedding >50% of limit
• DoC
Directive 84/500/EEC
44
Slide 43
Specific measures –substances
Slide 44
N-nitrosamines and N-nitrosatable substances
• in elastomers and rubber teats and soothers• Rules for migration testing and analysis• SML = 0.01 mg released N-nitrosamines /kg material• SML = 0.1 mg released N-nitrosatable substances /kg
material
Directive 93/11/EEC
45
Slide 45
Recycled plastics
Slide 46
Requirements• Scope: Mechanical recycling• Individual authorization of recycling process• Quality of input• Efficiency of the process of decontamination (challenge
test)• Restriction on the recyclate• Evaluation by EFSA of the recycling process• Requirements of the quality assurance system• Voluntary labelling• Declaration of compliance for the recyclate and for the
finished article
Recycled plastics
46
Slide 47
National Laws
Slide 48
National rules may derive:
• for all the EU Member States from harmonized EU rules
• for some EU Member States from pre-existing national laws or for new laws in sectors not yet harmonized
• The DG SANCO website gives information on the national laws of the Member States
National laws
47
Slide 49
FRANCE
Several décrets,...
BELGIUM GERMANY NETHERLANDS
BFR
ITALY
Arrêtés royaux 11/5/92 & 3/7/2005
SPAIN
Decreto 21/3/1973+Amendments
RESOLUCION 4/11/1982 warenwet
•Plastics•Rubbers •RCF••Paper&Paper&PaperboardPaperboard•Glass•Stainless steel
Macromolec.Compounds
Lebensm.und Futterm.
BGBI+
•53 BFRRecommend.(By Polymer
Type)+
Paper & Paper & PaperboardPaperboard
rec xxxvirec xxxvi
PlasticsCleaning agents
CoatingsElastomers&
rubbersIonisation
MetalsPaper&Paper&
PaperboardPaperboardRCF
Wood
PlasticsCeramicsCoatings
ElastomersGlassMetal
Paper&BoardPaper&BoardRCF
TextileWood
PlasticsTin
RCFPaper &
PaperboardCeramics
Glass
National laws – Member States
Slide 50
Other EC bodies and European organisationsinvolved in FCM control
48
Slide 51
JRC and EU Reference Laboratory
Risk management
(SANCO)
Official controls
Member State Authorities and
Enforcement Laboratories
As FCM activities 16 years Serving sectorial policies on release of substances from
food contact materials
As EU Reference Laboratory
Methods, migration data, scientific support for FCM
legislation
Ad-hoc contributions to EFSA for exposure assessment
Work
Supporting Regulation 882/2004 on official food controls Member State
authorities and enforcement Laboratories (NRLs)
Work
Slide 52
• Food and Veterinary Office (FVO)• checks on compliance with the requirements of EU food safety
and quality, animal health and welfare and plant health legislation within the European Union and on compliance with EU import requirements in third countries exporting to the EU
• contributes to the development of European Community policy in the food safety, animal health and welfare and plant health sectors
FVO
49
Slide 53
• Food and Veterinary Office (FVO)• contributes to the development and implementation of effective
control systems in the food safety, animal health and welfare and plant health sectors
• informs stakeholders of the outcome of its audits and inspections
• Each year the FVO develops an inspection programme, identifying priority areas and countries for inspection
FVO
Slide 54
• CoE is an European institution and is not the EU/EC• 48 countries adhere to the CoE
• These documents are not legally binding unless they are transposed into national laws
• However the majority of Member States recognise their validity in absence of EU and/or national rules
Council of Europe
50
Slide 55
• Resolution AP(89)1: colorants in plastics• Resolution AP(92)2: aids to polymerization
for plastics• Resolution AP(2002)1: paper and board• Guidelines: metals and alloys• Resolution AP(2004)1: coatings• Resolution AP(2004)2: cork • Resolution AP(2004)3: ion exchange resins
Inventory
Slide 56
• Resolution AP(2004)4: rubber• Resolution AP(2004)5: silicones• Resolution AP(2005)2: packaging inks• Guidelines: glass• Guidelines: paper kitchen towels and
napkins
Inventory
51
Slide 57
• The majority of the materials regulated by CoE are composed of:• Inventory Lists (less or more complete)• Rules for migration testing • Industrial GMP• Practical Guide
Council of Europe
Slide 58
• Composed of:• Substances authorised initially by EU countries, evaluated
by EFSA and authorized by EU measures (List 1)
• Substances approved by EU countries but not yet by EFSA and EU (appendix to List 1)
• Other substances requested by industry but not yet accompanied by the necessary documentation (List 2)
Inventory lists
52
Slide 59
• Rules for migration testing are inserted in a Technical Document which is approved only by the Committee and, then, easily amendable. These rules are often those of the EU for plastics but derogation are permitted, if technically justified
• "Practical Guide" is also a Technical Document the aim of which is to explain the Resolution and to give further detailed recommendations in its application
Council of Europe
Slide 60
• "GMP“ documents are prepared by industry but examined also by the Committee which inform all the stakeholders on how the product under consideration is manufactured
Council of Europe
53
Slide 61
Council of Europe ResolutionsExample – paper and board
Slide 62
Res. AP (2002)1: General requirements
Tech Doc No 1: List of substances (incomplete)
Tech Doc No 2: Guidelines on test conditions and methods of analysis
Tech Doc No 3: Guidelines for recycled fibres
Tech Doc No 4: The CEPI Guide for GMP
Tech Doc No 5: Practical Guide
Paper and board
54
Slide 63
• Inventory lists• SML and other restrictions are applicable• No OML• GMP• Suitable microbiological quality• No release of substances having an antimicrobial
effect
Paper and board
Slide 64
• Recycled fibres can be used (a) if it originates from specified qualities;
(b) if they are subject to appropriate processing and cleaning
(c) finished materials comply with the restrictions in the Resolution
Paper and board
55
Slide 65
• CEN standard methodology• Overall migration test methods
• Analytical methods (standards and technical specification) for testing compliance with SML and QM restrictions
CEN
Slide 66
• Rapid Alert System for Food and Feed (RASFF)• Was put in place to provide food and feed control authorities with
an effective tool to exchange information about measures taken responding to serious risks detected in relation to food or feed
• This exchange of information helps Member States to act more rapidly and in a coordinated manner in response to a health threat caused by food or feed
RASFF
56
Slide 67
Website on migration testing (JRC)http://ihcp.jrc.ec.europa.eu/our_labs/eurl_food_c_m
Website on risk assessments (EFSA)http://www.efsa.europa.eu/en/science/afc.html
Website on legislation (SANCO) http://ec.europa.eu/comm/food/food/chemicalsafety/foodcontact
/index_en.htm
Useful links
Council of Europehttp://www.coe.int/T/E/Social_Cohesion/soc-
sp/Public_Health/Food_contact/
Slide 68
New tool: Commission Databasehttps://webgate.ec.europa.eu/sanco_foods/main/?sector=FCM&auth=SANCAS
57
Slide 69
The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States
58
Lecture 3: Procedure and testing requirements for importing FCM in the EU.
Slide 1
Procedure and testing requirements for importing FCM in the EU
Catherine Simoneau
Slide 2
Overview
Regulatory requirements, particular related to testing, for importers who wish to import FCM into EU
Procedure for importers who intend to import FCM into EU
Requirements of testing laboratories for performing compliance testing to EU legislative requirements
Implementation timelines and details of the legislative requirements
Sampling plans for a shipping lot
59
Slide 3
Overview
Regulatory requirements, particular related to testing, for importers who wish to import FCM into EU
• All EU legislation described in the previous presentation is applicable
• Procedure for importers who intend to import FCM into EU• Declaration of compliance• Analytical test reports demonstrating compliance
Slide 4
How to export a product into Europe
Product (material type) fully regulated at EU level• Demonstrate compliance with the EU legislation previously
described
Product (material type) fully regulated at National level in one Member State
• Demonstrate compliance with the national legislation provided
Product (material type) fully regulated at National level in more than one Member State
• Demonstrate compliance with the national legislation of the country that has the most severe rules and apply the principle of mutual recognition
60
Slide 5
Principle of mutual recognition
Any product lawfully produced and marketed in one Member State must be admitted to the market of any other Member State
Member State can block under certain conditions the importation of products for
• protection of public health • environmental and other reasons
Slide 6
How to export a product into Europe
Product (material type) not regulated at EU or National level
accompany the product with adequate documentation showing that the product is safe
References documents such as FDA approval, other national recognised legislation and Council of Europe Resolutions, described later
61
Slide 7
Testing requirements
Requirements of the Framework Regulation
Requirements of the GMP Regulation
Is the material type specifically regulated at EU level?
If so which legislation is applicable?
Slide 8
Testing requirements
Have any restrictions been placed on the starting substances used to make the material or article?
Which tests should be carried out?
62
Slide 9
Requirements of the Framework Regulation
Labelling
Traceability
Declaration of compliance
Good manufacturing practice
Slide 10
Requirements of the GMP Regulation
GMP means those aspects of quality assurance which ensure that materials and articles are consistently produced and controlled to ensure conformity with the rules applicable to them and with the quality standards appropriate to their intended use by not endangering human health or causing an unacceptable change in the composition of the food or causing a deterioration in the organolepticcharacteristics thereof
63
Slide 11
Example – nylon kitchen utensils
Is the material type regulated at EU level by a specific measure?
• Yes, nylon is a plastic
If so which legislation is applicable?
• Framework Regulation (EC) No 1935/2004• Plastics Regulation EU No 10/2011• Regulation (EU) No 284/2011
Slide 12
Implementation of technical changes
Transitional provisions for compliance testing
• From January 1, 2013 to December 31, 2015, compliance documents should be based on migration testing using:
the food simulants established in the Regulation (EC) No. 10/2011 and the test conditions specified in 82/711/EEC, as amended, OR the test conditions established in the 10/2011
• From January 1, 2016, compliance documents should be based on migration testing using:
the food simulants and test conditions established in Regulation (EC) No. 10/2011
64
Slide 13
Requirements of testing laboratories
Validated analytical methods
Trained personnel
Participation in proficiency test schemes where available
Quality assurance
Accreditation (e.g. ISO 17025)
Slide 14
The content of this lecture does not necessarily represent the position of the European Commission or the EU Member
States
65
Lecture 4: Active and intelligent packaging
Slide 1
Active and intelligent packaging
Eddo J. Hoekstra
Joint Research Centre
The European Commission’s in-house science service
www.jrc.ec.europa.eu
Slide 2
food contact materials
smart materials
intelligent materials
active materials
•Monitor the condition of packaged food or the environment surrounding the food
•Release or absorb substances into or from the packaged food or the environment surrounding the food
•Extend shelf-life of packaged food
•Maintain/improve condition of packaged food
66
Slide 3
Benefits of smart materials
Traditional packaging• Passive barrier against microorganisms and chemicals
Smart Packaging• Reactive barrier against microorganisms and chemicals• Maintain/improve condition of packaged food
Colour
Organoleptic properties
Nutritional composition
Ripening
Deterioration
• Monitor the condition of packaged food or the environment surrounding the food
Freshness
Time-temperature
Slide 4
Waste and recycling
Longer shelf-life
Less food waste? Recycling?
Multi-material
Multi-layer plastic
67
Slide 5
Regulation Active and Intelligent materials
Slide 6
Active materials – absorbers
• Carbon dioxide
• Microbial growth
• Ethene
• Ripening
• Oxygen
• Microbial growth
• Water
• Deterioration of food
• Respiring food + fish/meat
Food
Food environment
Passive layer
Active layer
Environment
packaging
68
Slide 7
Active materials – releasers
• Carbon dioxide
• Ethanol
• Silver
• Sulphur dioxide
• grapes
• Anti-oxidants
• Flavours
• Tin
• simulate canned tomatoes
• Nitrogen
• foam on beer Food
Food environment
Passive layer
Active layer
Environment
packaging
anti-microbial
Slide 8
Smart but not active materials
Scavengers:
• Oxygen
• Acetaldehyde
• UV
Releasers:
• Heat
Beverages + microwave food
Material active or not?
• Depends on claim of producer
• Material should protect the food
– Not material – Not against environment
Food
Food environment
Passive layer
Active layer
EnvironmentPET
69
Slide 9
Placing on the market
• Suitable and effective for the intended purpose of use• Good Manufacturing Practice no transfer of their constituents
into food in quantities which could:– endanger human health – bring about an unacceptable change in the composition of
the food – bring about a deterioration in the organoleptic characteristics
thereof• Labelling, advertising and presentation of a material or article
shall not mislead the consumers.
Slide 10
Placing on the market
• Allowance of changes in the composition or organolepticcharacteristics of food on condition that the changes comply with the Community (or national) provisions applicable to food
• No misleading • masking the spoilage of food (active)• condition of the food (intelligent)
• Adequately labelling– to allow identification of non-edible parts
– DO NOT EAT (min font 3 mm) + label
– materials or articles are active/intelligent
70
Slide 11
Risk management of substances
Released active
substances intended to
be released
Substances classified as ‘mutagenic’, ‘carcinogenic’, or
‘toxic to reproduction’ Regulation (EC) No 1272/2008
Substances deliberately
engineered to nano-particle size
Authorisation procedure
Authorisation by relevant Community
provisions applicable to food
EU list
Substances not
actively released, grafted or behind FB
Substances used in components
which are not in direct contact with food and are separated
from the food by a functional
barrier
Substances falling within the scope of
Community or national provisions applicable to food,
which are grafted or immobilised in order
to have a technological effect
in the food
Discuss here the examples of the guideline on AIM
Slide 12
EU List substances
• Submission of applications for the safety assessment of substances to the European Food Safety Authority
• Public registry available with all substances having a valid application
• EFSA will deliver its opinion on all substances included in the register
• The Commission will establish the community list– Identity of the substance(s)– Function of the substance(s)– Reference number
If necessary:– Conditions of use of the substance(s) or component– Restrictions and/or specifications of use of the substance(s)– Conditions of use of the material to which the substance or
component is added or into which it is incorporated
Slide 13
71
‘
Non-Community List substances
Conditions of use of substances: • intended to be released into food• Grafted/immobilised on the active material with the intention of a
technological effect on food
– Full compliance with relevant Community and national provisions applicable to food and provisions in Regulation (EC) No 1935/2004
– Amount of release shall not be included in measured overall migration
– If substance is listed in e.g. plastic food contact material list, the amount released may exceed this specific restriction provided compliance with Community or national provisions for foods
Slide 14
Conditions of use of substances:• in indirect contact (behind functional barrier)
– Migration shall not exceed 0.01 mg/kg food– This limit applies to a group of substances if they are structurally and
toxicologically related– Not classified as mutagenic, carcinogenic or toxic to reproduction (EC
No 1272/2008)– Not nanoparticles
Non-Community List substances
‘
72
Slide 15
Released?
Check substance is approved under …
Flavour Regulation 1334/2008
Enzyme Regulation 1332/2008
Y N
Grafted or immobilised?
Y
Y
N
N
N
Y
Behind functional barrier?
Y
Y
N
Specific migration ≤0.01 mg/kg?
Compliance restrictions in EU list 450/2009?
N
N
Y
Compliance of substance in component AIM
Additive Regulation 1333/2008
Compliant
Compliance
Compl. prov. 1935/2004?
Compl. prov. national leg.?
Technol. effect on food?
Y
No active component
N
Not compliant
CMR or nano?
NY
compliance?
N
N
Substance released?
Y
Y
Slide 16
Risk management of anti-microbialsAnti-microbials in food contact materials
Application
Max residue limit in food
Active materialAuthorisation under 528/2012
Reg. 450/2009
Authorisation under 1333/2008
Use
Food preservativeSurface anti-microbial Process anti-microbial
Non-mandatory authorisation under 10/2011
Polymer production aid
Plastic FCMAuthorisation under national law
To be clarified yetApplicable 1/9/2013
5-chlo
ro-2-m
ethyl-
2H-
isothi
azol-3
-one,
mixtu
re
with
2-meth
yl-2H
isothi
azol-
3-one
(3:1)
in co
ating
, pap
er
Ag ze
olite
A in
PO, P
ET, P
C
73
Slide 17
Declaration of compliance
• All materials/components/substances • Issued by the business operator at every marketing stage in the
production chain− except when sold to consumers
• Appropriate documentation demonstrating compliance− Suitability− Effectiveness− Test conditions and results
− Calculations
− Other analysis an evidence on safety
− Reasoning
Slide 18
EFSA opinions on active substances
Register of substances with a valid application for authorisation
Moisture and liquid absorbers− Open-cell expanded polystyrene, talc, alkyl(C8-C22)sulphonic
acid salts for fresh fish, meat, poultry (EFSA J 2012-10-5-2746)
− Na carboxymethylcellulose, bentonite, KAl(SO4)2∙12H2O for not direct food contact (EFSA J 2012-10-10-2904)
74
Slide 19
EFSA opinions on active substances
Oxygen scavengers− Na borohydride, Pd acetate in plastic (EFSA J 2012-10-3-
2642)− activated carbon, H2O, Fe powder, kaolin calcined, sulphur
NaCl in sachet (EFSA J 2012-10-3-2643)− (terephthalic acid, dimethyl ester, polymer with 1,4-
butanediol, cyclized, polymers with glycidyl methacrylate, hydroxyl-terminated polybutadiene, methyl methacrylate and styrene) copolymer and cobalt stearate (catalyst) in PET (EFSA J 2012-10-10-2905)
− Fe(II) modified bentonite in plastic or sachet (EFSA J 2012-10-10-2906)
Slide 20
Entry into force and application
• 19 June 2009 – Entry into force
• From 19 December 2009 – Declaration of Compliance according to Regulation– Non-edible parts labelled according to Regulation
– labelled according to EC No 1935/2004 before 19/12/2009 marketing until exhaustion of stocks
• Date of application of Community List (≥ 2011)– < Authorise and use according to relevant Community
provisions applicable to food and EC No 1935/2004– > Composition requirements apply
75
Slide 21
Thank you!
Questions
http://ihcp.jrc.ec.europa.eu/our_labs/eurl_food_c_m
Slide 22
The content of this lecture does not necessarily represent the position of the European Commission or the EU Member States
76
Lecture 5: Testing compliance: migration testing for plastics
Slide 1
Testing compliance: migration testing for plastics
Catherine Simoneau
Slide 2
Overview
Food simulants and correspondence foods – simulants
Time – temperature conditions
Guidelines for interpretation of test conditions
Testing type
Overall migration testing
Testing for fatty contact
77
Slide 3
Testing strategies
Analysis of the material or article
Analysis of foods
Analysis of food simulants• The packaging can be tested for its suitability before use by
employing food simulants that are intended to mimic the migration properties of different categories of foods
• Introduced in the early-1980’s along with the rules for using simulants
Slide 4
screening tests
Alternative extraction tests indicated are permissible instead of migration tests with fatty food simulant when the results obtained in a ‘comparison test' show that the values are equal to or greater than those obtained in the test with simulant D
Any solvent/test conditions as long as the alternative extraction test result is higher
78
Slide 5
Food simulants
“Food simulant" means a test medium imitating food; in its behaviour the food simulant mimics migration from food contact materials
Designed to overestimate the migration into foods
Slide 6
Which simulant?
Regulation (EU) No 10/2011• Aqueous foods = Simulant A – 10% (v/v) aqueous ethanol
• Acidic foods (< pH 4.5) = Simulant B – 3% (w/v) aqueous acetic acid
• Alcoholic foods (< 20% alcohol) = Simulant C – 20% (v/v) aqueous ethanol
• Foods with an alcohol content of above 20% and for oil in water emulsions = Simulant D1 – 50% (v/v) aqueous ethanol
– Simulant D2 – vegetable oil
• Dry foods= Tenax
79
Slide 7
Slide 8
Assignment of simulants vs foods
80
Slide 9
Overall migration
Overall migration limit of 60 mg/kg
Because a test for overall migration using food simulants is entirely conventional – i.e. the test result depends on the method used – the standard test procedures have to be used and followed exactly
• CEN standards
Slide 10
Reg. (EU) No 10/2011: simplified scheme for OM
Test Contact time in days [d] or hours [h]
at Contact temperature in [ºC]
Intended food contact conditions
OM 1 10 d at 20°C Any food contact at frozen and refrigerated conditions.
OM2 10 d at 40°C Any long term storage at ambient temperature or below, including heating up to 70°C for up to 2 hours, or heating up to 100°C for up to 15 minutes.
OM3 2 h at 70°CAny contact conditions that include heating up to 70°C for up to 2 hours, or up to
100°C for up to 15 minutes, which are not followed by long term room or refrigerated temperature storage.
OM4 1 h at 100°C High temperature applications for all food simulants at temperature up to 100°C.
OM5 2 h at 100°C or at reflux or alternatively 1 h at 121°C High temperature applications up to 121°C.
OM6 4 h at 100°C or at reflux Any food contact conditions with food simulants A, B or C, at temperature exceeding 40°C.
OM7 2 h at 175°C High temperature applications with fatty foods exceeding the conditions of OM5.
81
Slide 11
Navigating options: OM
Screening approach
Solvent extraction #
Calculate totalmass of extractable
substances
Mass < OML?
Material compliant
Migration testing
Choose simulants(s)
Select exposure Select exposureconditions * conditions *
Perform migration Perform migration test test
Migration < OML? Migration test technically feasible?
Material Material compliant not compliant Migration < OML?
Perform tests with substitute simulants
Material Materialcompliant not compliant Migration < OML?
Material Materialcompliant not compliant
Yes No
A, B, C, D1 D2
Yes No Yes No
Yes No
Yes No
Overall migration
* Exposure conditions may be conventional conditions or accelerated test conditions using defined acceleration factors
# The results of solvent extraction tests may be used to demonstrate compliance with the legislative limit, provided that the result obtained in a comparison test shows that the value is equal to or greater than those obtained in the migration test with a conventional food simulant;
Slide 12
OM special cases of simulant assignment
82
Slide 13
Specific migration
• Positive list of monomers, other starting substances and additives permitted for use in the manufacture of plastic for food contact
• This list contains any limits on the migration of individual or groups of substances – limits that have been assigned following the toxicological assessment of these substances
Slide 14
Compliance with specific migration limits
Determination of the concentration of the substance(s) in the polymer
• Calculation of total transfer• Migration modelling
Determine the migration into food simulants
Determine the migration into foods
83
Slide 15
Concentration in the polymer
QM and QMA restrictions• e.g. Isocyanates• Volatiles• Reacts with food or food simulant
Demonstrate complete extraction• Polymer dissolution and subsequent precipitation• Successive solvent extraction• Selection of extraction solvent dependent on both the polymer
and the substance• cp,0
Slide 16
Migration modelling
Based on diffusion theory and a consideration of partitioning effects
• Diffusion coefficient of the migrant in the plastic (DP)• Partition coefficient of the migrant between the plastic and the
food or food simulant (KP,F)
84
Slide 17
Navigating options: SM
Screening approach
Solvent extraction # Parameters known for migration modelling?
Determine cP,0 and QM
Performmodelling
Calculate migrationassuming 100%
transferMigration < SML?
Migration < SML?
Materialcompliant
Material compliant
Migration testing
Choose simulants(s)
Select exposure Select exposureconditions * conditions *
Perform migration Perform migration test test
Migration < SML? Migration test technically feasible?
Material Materialcompliant not compliant Migration < SML?
Perform testswith substitute simulants
Material Materialcompliant not compliant Migration < SML?
Material Materialcompliant not compliant
Yes
Yes
Yes
No
No
No
A, B, C, D1 D2
Yes No Yes No
Yes No
Yes No
Specific migration –materials not in contact withfoods
* Exposure conditions may be conventional conditions or accelerated test conditions using defined acceleration factors
# Theresults of solvent extraction tests may be used to demonstrate compliance with the legislative limit, provided that the result obtained in a comparison test shows that the value is equal to or greater than those obtained in the migration test with a conventional
food simulant;
Not in core text of R10/2011
Slide 18
Test conditions: time of exposure
85
Slide 19
Test conditions: temperature of exposure
Slide 20
Long term storage
• 10 days at 20°C: Frozen foods
• 10 days at 40°C: refrigerated and frozen conditions including heating up to 70°C for up to 2 hours, or heating up to 100°C for up to 15 minutes
• 10 days at 50°C: storage time at cooled and frozen conditions including heating up to 70°C for up to 2 hours, or heating up to 100°C for up to 15 minutes and storage times of up to 6 months at room temperature
• 10 days at 60°C: long term storage above 6 months at room temperature and below including heating up to 70°C for up to 2 hours, or heating up to 100°C for up to 15 minutes
86
Slide 21
Specific cases
Contact conditions generally recognized as ‘more severe’
Contact with foodstuffs at any condition of time and temperature
Contact with foodstuffs at room temperature or below for an unspecified period
Contact in a microwave oven
Slide 22
Specific cases
Contact conditions causing changes in physical or other properties
Contact for less than 15 min at temperatures between 70°C and 100°C
87
Slide 23
Now in practice: OM and SM
Slide 24
Migration testing
Single face immersion cell
Total immersion test
1 dm2 cutting template
Pouch testing
Article filling
Support for strips
88
Slide 25
Double face testing by immersion
Single surface testing using
pouches
Single surface testing using cells
article filling
1 dm2
equilibrated at Tº
S1 S2 S3 B1 B2
+ +
S1 S2 S3 B1 B2
+ simulant at Tº
filler plug
clamp screw
clamp bar
rubber mat
food simulant
lid
base plate
sealing ring
Type A (Pira cell) Type B (TNO cell)
cell at Tº + liquid at T
wire gauze support
simulant
EXPOSURE (t, T)
pouch holder at Tº
hole
10 x 10 cm
seal pouch: sides in contact with simulant
facing
90 ¼C
120
175
11
60
120
Migration testing
Slide 26
Testing set-ups for time temperature exposures
Foods in glass single face cell (e.g. rigid
films)
Single cell and simulant
Total immersion in olive oil
89
Slide 27
Sampling and testing
Slide 28
Sampling – overall migration
Overall migration• Four test specimens for the test for each simulant• Two additional test specimens to determine loss of volatiles when
testing using simulant D• One additional test specimen to determine the suitability of olive
oil as the fatty food simulant and triheptadecanoin as the internal standard
• If the articles are an irregular shape then another two test specimens are required to determine the surface area
90
Slide 29
Sampling – specific migration
Specific migration• Not well defined• Recommendations in the EURL-NRL guidelines are based on
Directive 2004/16/EC laying down the sampling methods and the methods of analysis for the official control of the levels of tin in canned foods
Slide 30
Selection of test conditions
Compliance testing is SIMULATION of WORST case migration into food
Appropriate selection of test conditions is VERY important to obtain COMPARABLE test results and correct evaluation food contact materials
91
Slide 31
Standard methods
Slide 32
Recognised methods
“Community methods” = methods laid down in the legislation (only for ceramics)
Internationally recognized: CEN • Reliable, collaboratively tested, to be used in case of dispute• EN 1186 Overall migration plastics• EN 13130 Specific migration plastics• TS 14235 polymeric coatings… and others
Link CEN: http://www.cen.eu/cenorm/standards_drafts/index.asp
Other technical specifications• Directives (ceramics, vinyl chloride)• CoE guidelines, national legislations or recommendations
92
Slide 33
CEN methods – overall migrationStandard reference Title Plastics Materials and articles in contact with foodstuffs - Plastics - EN 1186-1:2002 Part 1: Guide to the selection of conditions and test methods for overall migration EN 1186-2:2002 Part 2: Test methods for overall migration into olive oil by total immersion EN 1186-3:2002 Part 3: Test methods for overall migration into aqueous food simulants by total immersion EN 1186-4:2002 Part 4: Test methods for overall migration into olive oil by cell EN 1186-5:2002 Part 5: Test methods for overall migration into aqueous food simulants by cell EN 1186-6:2002 Part 6: Test methods for overall migration into olive oil using a pouch EN 1186-7:2002 Part 7: Test methods for overall migration into aqueous food simulants using a pouch EN 1186-8:2002 Part 8: Test methods for overall migration into olive oil by article filling EN 1186-9:2002 Part 9: Test methods for overall migration into aqueous food simulants by article filling EN 1186-10:2002 Part 10: Test methods for overall migration into olive oil (modified method for use in cases where incomplete extraction of olive oil occurs) EN 1186-11:2002 Part 11: Test methods for overall migration into mixtures of C-labelled synthetic triglycerides EN 1186-12:2002 Part 12: Test methods for overall migration at low temperatures EN 1186-13:2002 Part 13: Test methods for overall migration at high temperatures EN 1186-14:2002 Part 14: Test methods for 'substitute tests' for overall migration from plastics intended to come into contact with fatty foodstuffs using test media iso-octane and 95 % ethanol EN 1186-15:2002 Part 15: Alternative test methods to migration into fatty food simulants by rapid extraction into iso-octane and/or 95 % ethanol
Slide 34
5. Slow evaporation of liquid (hot plate)
4. Removal of specimens, take residual liquid
1. Glassware weight empty (m1)
CEN methods – Overall migration aqueous• Exposure to test
simulant, evaporation to dryness, weight of residue
L1S1 S2 S3 B1B2
S1 S2 B1S3 B2mbS1 mbS2 mbS3 mbB1 mbB2
Overall migration:
determined by the mass of residue after evaporation of the food simlant
M = (ma - mb) x 1000
mg/dm2 S
S1 S2 B1S3 B2
2. Sample preparationx 7 samples
3. Exposure to food simulant (t, T)
simulant
S1 S2 S3 B1 B2L06. oven-dessicator to
weight final mass (m2)S1 S2 B1S3 B2
mbS1 mbS2 mbS3 mbB1 mbB2
S1 S2 B1S3 B2
Valid and reproducible
results require expertise
93
Slide 35
CEN methods –Overall migration oil
6. GC-FID determination of absorbed oil by FAME -> m3
3. Remove free oil & weight sample (m2)
2. Exposure to food simulant (t, T)
1. Sample weight before exposure (m1)
5. Derivatisation of absorbed oil byfatty acid methyl esters (FAME)
4. Extraction of absorbed oil
(soxhlet)
simulant
H20
H20H20H20
S1 S2 S3 B2 E1 E2S4 B1
x 7 samples record masses: ma
repeat FAME with 6
standards 0-50 mg oil (C17 spiked) for calibration
curve
7. Overall migration:
Determined by weight loss of specimen
M = (ma - (mb - mc )) x 1000
mg/dm2 S
Valid and reproducible
results require
expertise
E L Bradley, Hong Kong Seminar May 2011
empty tubes: adjust for loss of volatiles
Slide 36
Check points –Overall migration in oil
Stable weight of test sample (conditioning of sample)
Test temperature according of the analytical tolerances
Extraction efficiency of the oil
Linearity of calibration curve
C18/C16 ratio of extracted oil – check for interferences
Individual results must be within analytical tolerance
94
Slide 37
Specific migration
Determination of quantity after migration of a specific substance (targeted analyses)
3 steps: extraction, clean-up (if necessary), determination
Analytical approach depends on:• Volatility and polarity of the substance • Nature of food simulant• Level of determination• Functional groups of the substance
Slide 38
Specific migration
Lowest sensitivity (non-detectable): 10 µg subst / kg food
Source of analytical methods: • CEN (series EN 13130 for plastics)• EU Reference Laboratory web site:
95
Slide 39
SM: plastics (1)
Standard reference Title
Plastics Materials and articles in contact with foodstuffs - Plastics substances subject to limitation -
EN 13130-1:2004 Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food
simulants and the determination of substances in plastics and the selection of conditions of exposure
to food simulants
EN 13130-2:2004 Part 2: Determination of terephthalic acid in food simulants
EN 13130-3:2004 Part 3: Determination of acrylonitrile in food and food simulants
EN 13130-4:2004 Part 4: Determination of 1,3-butadiene in plastics
EN 13130-5:2004 Part 5: Determination of vinylidene chloride in food simulants
EN 13130-6:2004 Part 6: Determination of vinylidene chloride in plastics
EN 13130-7:2004 Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants
EN 13130-8:2004 Part 8: Determination of isocyanates in plastics
CEN/TS 13130-9:2005 Part 9: Determination of acetic acid, vinyl ester in food simulants
CEN/TS 13130-10:2005 Part 10: Determination of acrylamide in food simulants
Slide 40
SM: plastics (1)
Standard reference Title
Plastics Materials and articles in contact with foodstuffs - Plastics substances subject to limitation -
CEN/TS 13130-11:2005 Part 11: Determination of 11-aminoundecanoic acid in food simulants
CEN/TS 13130-12:2005 Part 12: Determination of 1,3-benzenedimethanamine in food simulants
CEN/TS 13130-13:2005 Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants
CEN/TS 13130-14:2005 Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulants
CEN/TS 13130-15:2005 Part 15: Determination of 1,3-butadiene in food simulants
CEN/TS 13130-16:2005 Part 16: Determination of caprolactam and caprolactam salt in food simulants
CEN/TS 13130-17:2005 Part 17: Determination of carbonyl chloride in plastics
CEN/TS 13130-18:2005 Part 18: Determination of 1,2-dihydroxybenzene, 1,3-dihydroxybenzene, 1,4-dihydroxybenzene, 4,4'-
dihydroxybenzophenone and 4,4'dihydroxybiphenyl in food simulants
CEN/TS 13130-19:2005 Part 19: Determination of dimethylaminoethanol in food simulants
96
Slide 41
SM: plastics (2), paper and board
Standard reference Title
Plastics Materials and articles in contact with foodstuffs - Plastics substances subject to limitation -
CEN/TS 13130-20:2005 Part 20: Determination of epichlorohydrin in plastics
CEN/TS 13130-21:2005 Part 21: Determination of ethylenediamine and hexamethylenediamine in food simulants
CEN/TS 13130-22:2005 Part 22: Determination of ethylene oxide and propylene oxide in plastics
CEN/TS 13130-23:2005 Part 23: Determination of formaldehyde and hexamethylenetetramine in food simulants
CEN/TS 13130-24:2005 Part 24: Determination of maleic acid and maleic anhydride in food simulants
CEN/TS 13130-25:2005 Part 25: Determination of 4-methyl-1-pentene in food simulants
CEN/TS 13130-26:2005 Part 26: Determination of 1-octene and tetrahydrofuran in food simulants
CEN/TS 13130-27:2005 Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulants
CEN/TS 13130-28:2005 Part 28: Determination of 1,1,1-trimethylolpropane in food simulants
Slide 42
Detection of migratable substances
Range of substances with migration limits assigned means in turn that a range of analytical methods are deployed in testing;
• Headspace GC-MS for the volatiles• GC-MS for the semi-volatiles• LC-MS for the non-volatiles and the polar residues
The detection level needed depends on the toxicological or organoleptic properties
97
Slide 43
Other considerations
Simulant D (and its substitutes) reduction factor• numbers, 2 to 5, which may be applied to the result of the
migration tests relevant to certain types of fatty foodstuffs and which is conventionally used to take account of the greater extractive capacity of the simulant for such foodstuffs
Slide 44
Other considerations
Fat reduction Factor (FRF)
The exposure to substances migrating predominantly into fatty food (lipophilic substances) was previously based on the general assumption that a person ingests daily 1 kg of food. However, a person ingests at most 200 g of fat on a daily basis
• FRF applicable to lipophilic substances• Applicable substances listed in Directive 2002/72/EC, as amended
98
Slide 45
Testing for fatty contact
For certain foodstuffs if it can be demonstrated that the foodstuff does not make “fatty contact” with the plastic then testing with simulant D is not required
• This is determined by placing food in contact with a polyethylene film containing a fat-soluble fluorescent dye. The degree of transfer of the dye from the film is related to the extent of fatty contact made, and is used to determine whether simulan