CEN/TR 15356-1:2006
(Main)Validation and interpretation of analytical methods, migration testing and analytical data for materials and articles in contact with food - Part 1: General considerations
Validation and interpretation of analytical methods, migration testing and analytical data for materials and articles in contact with food - Part 1: General considerations
This Technical Report gives guidance in support of Directives adopted by the European Union in the Food Contact Materials Sector and is intended to aid Food Control Authorities and industry enforce and comply with those Directives.
Validierung und Interpretation analytischer Verfahren, Migrationsprüfung und analytischer Daten von Werkstoffen und Bedarfsgegenständen in Kontakt mit Lebensmitteln - Teil 1: Allgemeine Betrachtungen
Validation et interprétation des méthodes d'analyse, essais de migrations et données analytiques des matériaux et objets en contact avec les denrées alimentaires - Partie 1 : Considérations générales
Validacija in interpretacija analitskih metod, migracijsko preskušanje in analitski podatki za materiale in predmete v stiku z živili – 1. del: Splošne ugotovitve
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2006
Validacija in interpretacija analitskih metod, migracijsko preskušanje in analitski
podatki za materiale in predmete v stiku z živili – 1. del: Splošne ugotovitve
Validation and interpretation of analytical methods, migration testing and analytical data
for materials and articles in contact with food - Part 1: General considerations
Validierung und Interpretation analytischer Verfahren, Migrationsprüfung und
analytischer Daten von Werkstoffen und Bedarfsgegenständen in Kontakt mit
Lebensmitteln - Teil 1: Allgemeine Betrachtungen
Validation et interprétation des méthodes d'analyse, essais de migrations et données
analytiques des matériaux et objets en contact avec les denrées alimentaires - Partie 1 :
Considérations générales
Ta slovenski standard je istoveten z: CEN/TR 15356-1:2006
ICS:
67.250
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
TECHNICAL REPORT
CEN/TR 15356-1
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
March 2006
ICS 13.060.20; 23.060.50
English Version
Validation and interpretation of analytical methods, migration
testing and analytical data for materials and articles in contact
with food - Part 1: General considerations
Validation et interprétation des méthodes d'analyse, essais Validierung und Interpretation analytischer Verfahren,
de migrations et données analytiques des matériaux et Migrationsprüfung und analytischer Daten von Werkstoffen
objets en contact avec les denrées alimentaires - Partie 1 : und Bedarfsgegenständen in Kontakt mit Lebensmitteln -
Considérations générales Teil 1: Allgemeine Betrachtungen
This Technical Report was approved by CEN on 16 January 2006. It has been drawn up by the Technical Committee CEN/TC 194.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,
Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 15356-1:2006: E
worldwide for CEN national Members.
Contents Page
Foreword. 3
Introduction . 4
1 Scope. 6
2 Form of regulations . 6
3 Terms and definitions. 7
4 Analytical tolerances . 10
5 Limits. 12
6 Existing general legislation . 14
7 Difficulties with present situation regarding method validation. 17
8 Analytical interpretation of results and limits. 19
9 Single laboratory method validation - General protocol. 23
10 Single laboratory and second laboratory validation - For the food contact
materials sector. 23
11 FDA requirements with respect to validation of analytical methods . 25
12 Recovery . 25
13 Reference materials. 27
14 Costs . 28
15 Sampling . 29
16 Enforcement . 30
17 Conclusions. 30
Annex A (informative) Food contact materials and articles: EU legislation. 31
Annex B (informative) List of methods currently available. 37
Annex C (informative) Codex proposed draft guidelines on measurement uncertainty. 39
Annex D (informative) Characteristics of available certified reference materials. 41
Bibliography . 42
Foreword
This document (CEN/TR 15356-1:2006) has been prepared by CEN /TC 194, "Utensils in contact with
food", the secretariat of which is held by BSI.
Introduction
0.1 Requirement for validation of analytical methods for enforcement of Directives
[1]
Regulation (EC) No. 1935/2004 has laid down the requirements that may be included in specific
Directives to protect human health. It allows for specific Directives to set overall migration limits and
specific limits on the migration of certain constituents or groups of constituents into foodstuffs.
[2] [3]
Commission Directive 90/128/EEC and its subsequent amendments (e.g. ) introduced specific
migration limits for more than 300 substances. A consolidation of these directives has since been
[4]
issued as Commission Directive 2002/72/EC . In addition, some substances are subject to a
maximum permitted quantity of the residual substance in the material or article. Some substances are
subject to group limits. Continuously, additional substances are being evaluated and added to the
Directive.
New technical dossiers are being prepared for substances which could eventually be listed in future
amendments to Directive 2002/72/EC. Methods of control will be required for the majority of the
abovementioned substances.
[5]
The two Food Control Directives (European Council Directive 89/397/EEC and Council Directive
[6]
93/99/EEC ) require that methods used for control purposes must be correctly and fully validated. So
far only the methods developed by CEN as parts of EN 13130 have been so validated. Methods
developed in the project sponsored by DG Research (SM&T project, MAT1-CT92-0006,
"Development of Methods of Analysis for Monomers") have only been validated by two competent
laboratories. Most methods from technical dossiers have only limited validation data at best.
This Technical Report considers the background to whether or not acceptable validation of analytical
methods could be achieved faster and at less cost. The Technical Report also considers the need for
validation of the whole test procedure for enforcement purposes, for compliance purposes, and for the
creation of data for risk assessment purposes. It should be noted that the considerations apply to both
overall as well as specific migration.
The list of current legislation currently adopted by the Commission is given in Annex A.
The list of current methods adopted by CEN/TC 194/SC 1 is given in Annex B.
0.2 Variability in the migration contact stage
The determination of migration from plastics is quite unlike other measurement tasks in ensuring food
safety and quality. Reliable measurements depend upon more than simply having validated analytical
methods for measuring chemical concentrations in foods. The Directives allows that, as an alternative
to the analysis of foodstuff itself, migration testing can be carried out with food simulants applied
under conditions which simulate actual use of the plastic material or article with food. This introduces
many potential sources of variability in the final migration value. These are discussed in Clause 8.
0.3 Quality of data submitted for risk assessment purposes
Migration data is usually an important part of the petition submitted for a risk assessment carried out
by the Scientific Committee on Food (since 2003, by the European Food Safety Authority, EFSA). For
new substances it is unlikely that a fully validated method in food simulants will exist. A single
laboratory (in-house) system of validation is required as part of the demonstration that the data
submitted is of adequate quality. For example, validation of a method’s intended use, the
determination of accuracy and precision, usually involves replicate analyses of appropriate matrices
spiked with known amounts of the additive at concentrations similar to those encountered in the
migration studies and determination of the percentage recovery of the spiked additive.
Where data are supplied to other authorities, e.g. the US-FDA, the data has to be applicable and
acceptable to those authorities.
Even when a validated method exists there is still the need for the laboratory carrying out the test to
ensure the migration testing carried out within the laboratory does not suffer from excessive error. The
possibility of error may be reduced by taking part in proficiency testing schemes. Proficiency testing
schemes aim to assess the competence of laboratories to carry out migration testing. At present there
is at least one scheme which is known to operate in this area. This is the Food Analysis Performance
Assessment Scheme (FAPAS) operated by the FAPAS Secretariat, Central Science Laboratory, Sand
Hutton, York (UK).
Laboratories carrying out these methods will also be able to demonstrate their general competence by
being accredited to EN ISO/IEC 17025:2005, which is administered by the appropriate Accreditation
Agencies in the European Countries. For overall migration testing, samples of plastics with known
overall migration values are available from the IRMM, Geel, Belgium. Spectra and a table of physical
properties of the monomers and additives listed in Directives have been published to assist ensuring
[7], [8]
that substances used for calibration are of adequate and known purity .
1 Scope
This Technical Report gives guidance in support of Directives adopted by the European Union in the
Food Contact Materials Sector and is intended to aid Food Control Authorities and industry enforce
and comply with those Directives.
2 Form of regulations
2.1 General
The EU Directives on food contact plastics, provide for various types of quantitative restrictions i.e.
specific migration limits (SML, expressed as mg (of substance) /kg of food), overall migration limit
(OML, expressed as mg/kg of food or mg/dm of surface) and maximal quantity of the substance in
the finished plastic article referred either to the quantity of article (QM, expressed as mg/kg of article)
or to area of the surface in contact with the foodstuffs (QMA, expressed as mg/dm² of surface). The
determination of these quantities implies various procedural steps e.g. sampling, migration tests with
different experimental conditions (OML, SML) or extraction (QM, QMA) as well the usual multi-step
analytical determination. Each of these steps is subject to a certain variability and an overall variability
will affect the value found by one laboratory (repeatability) or by more than one laboratories
(reproducibility). In the past at the level of the Standing Committee for Foodstuffs a discussion took
place on the method of analysis for vinyl chloride. The Commission proposed then that the variability
should be expressed as "Reproducibility" but the majority of Member States were in favour of the
"Repeatability". Therefore the Commission services decided to avoid any further scientific discussion
on this issue and decided to propose a new term, "Analytical Tolerance" which shall comprise the
variability due to all the above-mentioned procedural steps. Until now no Member States objected to
this choice and no fundamental problems were raised from its application. Three options have been
chosen by the Commission services as regards the various existing quantitative restrictions:
a) restrictions affected by a specified analytical tolerance,
b) restrictions affected by an unspecified analytical tolerance, and
c) restrictions not affected by any analytical tolerance.
The three options and their background are explained in 2.2, 2.3 and 2.4.
2.2 Restriction and specified analytical tolerance
This case applies to the overall migration limit, where the value of the OML in fatty simulants
(60 mg/kg (ppm) or 10 mg/dm ) is accompanied by an analytical tolerance of 20 mg/kg (ppm)
(or 3 mg/dm ). In this case the variability should be added to the limit value and, only if the value
found is greater than 80 mg/kg (ppm) (=60+20) or 13 mg/dm (=10+3), the article is considered not in
compliance with the Directive. The choice to increase the OML by the value of the tolerance was due
to the variability of the analysis.
NOTE This approach has the disadvantage that as the variability of sampling and analytical procedures
becomes less, the overall limit becomes, effectively greater. However it is possible to change the value of t
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.