SIST-TP CEN/TR 16059:2011

SLOVENSKI STANDARD
SIST-TP CEN/TR 16059:2011
01-marec-2011
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Food analysis - Performance criteria for single laboratory validated methods of analysis
for the determination of mycotoxins
Untersuchung von Lebensmitteln - Leistungskriterien für Einzel-labor validierte Verfahren
zur Bestimmung von Mykotoxinen
Analyse des produits alimentaires - Critères de performance des méthodes validées
monolaboratoires d'analyse des mycotoxines
Ta slovenski standard je istoveten z: CEN/TR 16059:2010
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
SIST-TP CEN/TR 16059:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TP CEN/TR 16059:2011

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SIST-TP CEN/TR 16059:2011


TECHNICAL REPORT
CEN/TR 16059

RAPPORT TECHNIQUE

TECHNISCHER BERICHT
October 2010
ICS 07.100.30
English Version
Food analysis - Performance criteria for single laboratory
validated methods of analysis for the determination of
mycotoxins
Analyse des produits alimentaires - Critères de Untersuchung von Lebensmitteln - Leistungskriterien für
performance des méthodes validées monolaboratoires Einzel-labor validierte Verfahren zur Bestimmung von
d'analyse des mycotoxines Mykotoxinen


This Technical Report was approved by CEN on 19 June 2010. It has been drawn up by the Technical Committee CEN/TC 275.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, 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: Avenue Marnix 17, B-1000 Brussels
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 16059:2010: E
worldwide for CEN national Members.

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Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Terms and definitions .5
3 General criteria for analytical methods for mycotoxins . 10
4 Specific criteria for analytical methods for mycotoxins . 11
Bibliography . 14

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Foreword
This document (CEN/TR 16059:2010) has been prepared by Technical Committee CEN/TC 275 “Food
analysis - Horizontal methods”, the secretariat of which is held by DIN.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
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Introduction
Within the European Union, regulatory and scientific interest in mycotoxins has undergone a development in
the last decade from autonomous national activity towards more EU-driven activity with a structural and
network character. Harmonized EU limits now exist for several dozens of mycotoxin-food combinations, and
this number will further grow in the coming years. The direct or indirect influence of European organizations
and programmes on the EU mycotoxin regulatory developments has become significant. For example the
position of CEN with regards to mycotoxin regulations has been strengthened as a consequence of the
European Commission’s “Mandate for standardization addressed to CEN in the field of methods of analysis
for mycotoxins in food“ [1]. The new mandate falls within the framework of regulation EC no 882/2004 [2]. This
regulation stipulates that methods for sampling and analysis used in the context of official control shall comply
with relevant Community rules or, if no such rules exist, with internationally recognized rules or protocols, for
example those that CEN has accepted. The view of the European Commission on CEN standards is clear:
“The establishment of standardized methods of analysis is of utmost importance to guarantee a uniform
application and control of the European legislation in all Member States. Standardized methods of analysis
are an indispensable element in guaranteeing a high level of food safety”. In the annex of the mandate a
number of methods of analysis, for which standardized procedures are necessary, have been specifically
mentioned. In addition to these tasks, a special task has been indicated: The preparation of a review of
updates and extended performance criteria for methods of analysis of mycotoxins.
The objective is to produce a complementary version of CEN report, CR 13505, Food analysis ― Biotoxins ―
Criteria of analytical methods of mycotoxins [3], which has been the basis for stipulating performance criteria
for mycotoxin methods in current EU legislation.
Complementary to the currently accepted approach, where method performance statistics are obtained from
formal interlaboratory validation studies as defined within CR 13505, the concept presented in this document
has single-laboratory validation as the primary source of method performance statistics.
The highly preferred option, by default, is for all standards developed through CEN/TC 275/WG 5 "Biotoxins"
to contain method performance data generated from formal interlaboratory validation studies undertaken to
either the Harmonised IUPAC Protocol (1995) or ISO 5725:1994. However, it is recognised that in some
circumstances the interlaboratory validation study approach is impracticable. Additional method performance
criteria should be developed in order to aid laboratories undertaking official food or feed control and also to
help guide CEN/TC 275/WG 5 when considering the standardisation of methods supported by single-
laboratory validation data. This document is not intended to replace CR 13505:1999. It will be complementary.
Some of the criteria in this document could have influence on the conclusions regarding the acceptability of
validation studies that have already been performed and that were the basis for recent CEN standards on
various mycotoxins. Therefore a comparison was made using criteria for single-laboratory validation instead of
criteria for interlaboratory validated methods. Validation parameters such as RSD , RSD, and
WLR r
trueness/recovery were considered. A large majority of these CEN standards still show acceptable
performance using the criteria written down in this document.
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1 Scope
This Technical Report gives criteria for single laboratory validated methods of analysis for the determination of
mycotoxins. The criteria and topics covered are accuracy, trueness, recovery, precision, measurement
uncertainty, selectivity, applicability, linearity, limit of detection, limit of quantification, sensitivity, ruggedness,
specificity. This report also contains information on terms and definitions, validation, standardization
procedures and interlaboratory studies by international organizations (e.g. AOAC, CEN, ISO, IUPAC, IDF).
Confirmatory methods and screening methods are described. The validation criteria specified for mycotoxins
in general are given.
2 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
2.1
accuracy
closeness of agreement between a test result and the accepted reference value
NOTE The term accuracy, when applied to a set of test results, involves a combination of random components and a
common systematic error or bias component.
[ISO 5725-1:1994, see [4]]
2.2
trueness
closeness of agreement between the average value obtained from a large series of test results and an
accepted reference value
[ISO 5725-1:1994, see [4]]
2.3
recovery
c −c
f, meas unf, meas
recovery = ×100 % (1)
c
known
where
c is the measured concentration (mass fraction) in fortified material;
f, meas
c is the measured concentration (mass fraction) in unfortified material;
unf, meas
c is the known increment in concentration (mass fraction)
known
NOTE 1 The amount added should be a substantial fraction of, or more than, the amount present in the unfortified
material. Ideally, the unfortified material should contain no measurable level of the analyte under test.
NOTE 2 A true or assigned value is known only in cases of spiked or fortified materials, certified reference materials, or
by analysis by another (presumably unbiased) method. The concentration (mass fraction) in the unfortified material is
obtained by direct analysis or by the method of standard additions. In other cases, there is no direct measure of bias, and
consensus values derived from the collaborative study itself often can be used for the reference point.
[CR 13505:1999, see [3]]
2.4
precision
closeness of agreement between independent test results obtained under stipulated conditions
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NOTE 1 Precision depends only on the distribution of random errors and does not relate to the true value, conventional
true value or specified value.
NOTE 2 The measure of precision is usually expressed in terms of imprecision and computed as a standard deviation
of the test results. Less precision is reflected by a larger standard deviation.
NOTE 3 Independent test results means results obtained in a manner not influenced by any previous result on the
same or similar test object. Quantitative measure of precision depends critically on the stipulated conditions. Repeatability
and reproducibility conditions are particular sets of extreme conditions.
[ISO 5725-1:1994, see [4]]
2.5
repeatability
precision under repeatability conditions
[ISO 5725-1:1994, see [4]]
2.6
repeatability conditions
conditions where independent test results are obtained with the same method on identical test items in the
same laboratory by the same operator using the same equipment within short intervals of time
[ISO 5725-1:1994, see [4]]
2.7
within-laboratory reproducibility
precision under within-laboratory reproducibility conditions
2.8
within-laboratory reproducibility conditions
conditions where test results are obtained with the same method on identical test items on different days with
different operators using different equipment
[ISO 5725-1:1994, see [4]]
2.9
reproducibility
precision under reproducibility conditions
NOTE 1 It is a measure of the dispersion of the distribution of test results under reproducibility conditions.
NOTE 2 Similarly "reproducibility variance" and "reproducibility coefficient of variation" could be defined and used as
measures of the dispersion of the test results under reproducibility conditions.
[ISO 5725-1:1994, see [4]]
2.10
reproducibility conditions
conditions where test results are obtained with the same method on identical test items in different
laboratories with different operators using different equipment
[ISO 5725-1:1994, see [4]]
2.11
Horwitz ratio
HorRat
normalized performance parameter indicating the acceptability of methods of analysis with respect to among-
laboratory precision (reproducibility)
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NOTE 1 It is the ratio of the observed relative standard deviation among laboratories calculated from the actual
performance data, RSDR (%), to the corresponding predicted relative standard deviation calculated from the Horwitz
equation. It is more or less independent of analyte, matrix, method, and time of publication.
NOTE 2 See [5].
2.12
RSD
r
relative standard deviation, calculated from results generated under repeatability conditions
S
r
RSD = ×100 % (2)
r
c
mean
where
S is the standard deviation, calculated from results generated under repeatability conditions;
r
c is the mean concentration (mass fraction)
mean
[Based on CR 13505:1999, see [3]]
2.13
RSD
WLR
relative standard deviation, calculated from results generated under within-laboratory reproducibility conditions
(WLR)
S
WLR
RSD = ×100 % (3)
WLR
c
mean
where
S is the standard deviation, calculated from results generated under within-laboratory
WLR
reproducibility conditions;
c is the mean concentration (mass fraction)
mean
2.14
RSD
R
relative standard deviation, calculated from results generated under reproducibility conditions
S
R
RSD = ×100 % (4)
R
c
mean
where
S is the standard deviation, calculated from results generated under reproducibility conditions;
R
c is the mean concentration (mass fraction)
mean
[Based on CR 13505:1999, see [3]]
2.15
measurement uncertainty
parameter associated with the result of a measurement, that characterises the dispersion of the values that
could reasonably be attributed to the measurand
NOTE 1 See [6].
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NOTE 2 Uncertainty of measurement comprises, in general, many components. Some of these components may be
estimated on the basis of the statistical distribution of the results of a series of measurements and can be characterized by
standard deviations. Estimates or other components can only be based on experience or other information.
NOTE 3 Uncertainty should be distinguished from an estimate attached to a test result which characterizes the range
of values within which the expectation is asserted to lie. This latter estimate is a measure of precision rather than of
accuracy and should be used only when the true value is not defined.
2.16
selectivity
degree to which a method can quantify the analyte accurately in the presence of interferences
NOTE 1 See [7].
NOTE 2 Ideally, selectivity should be evaluated for any important interferences likely to be present. It is particularly
important to check interferences that are likely, on chemical principles, to respond to the test. As a general principle,
selectivity should be sufficiently good for any interferences to be ignored.
2.17
applicability
description of analytes, matrices and concentrations (mass fractions) to which the method can be applied
NOTE See [8].
2.18
linearity
ability (within a given range) of an analytical procedure to obtain test results which are directly proportional to
the mass (fraction) of analyte in the sample
NOTE See [9].
2.19
limit of detection
LOD
smallest mass (fraction) of analyte in the test sample that can be reliably distinguished from zero
NOTE 1 See [7].
NOTE 2 For analytical systems where the validation range does not include or approach it, the detection limit does not
need to be part of a validation
NOTE 3 Despite the apparent simplicity of the idea, the whole subject of the detection limit is beset with problems
outlined below:
 There are several possible conceptual approaches to the subject, each providing a somewhat different definition of
the limit. Attempts to clarify the issue seem ever more confusing.
 Although each of these approaches depends of an estimate of precision at or near zero concentration (mass
fraction), it is not clear whether this should be taken as implying repeatability conditions or some other condition for
the estimation.
 Unle
...