Animal feeding stuffs - Methods of sampling and analysis - Performance criteria for single laboratory validated and ring-trial validated methods of analysis for the determination of mycotoxins

This document specifies performance criteria for the selection of single-laboratory validated or collaborative study validated methods of analysis of mycotoxins in feed. The terms and definition of the relevant parameters for method validation are included. The performance requirements and characteristics are provided. This document could serve as a guide:
— to assess the quality of new European Standard methods under validation;
— to review the quality of previous collaborative trials;
— to confirm the extension of the scope of an already published European Standard applied to other analyte concentrations or matrices; or
— to evaluate the fitness-for-purpose of single-validated methods.
The performance criteria can apply to methods dedicated to the determination of mycotoxins.

Futtermittel - Probenahme und Untersuchungsverfahren - Leistungskriterien für laborintern validierte und im Ringversuch validierte Analysemethoden zur Bestimmung von Mykotoxinen

Dieses Dokument legt Leistungskriterien für die Auswahl von in Einzellaboratorien validierten oder in Laborvergleichsuntersuchungen validierten Analyseverfahren für Mykotoxine in Futtermitteln fest. Enthalten sind die Begriffe der relevanten Parameter für die Verfahrensvalidierung. Die Leistungsanforderungen und  merkmale werden zur Verfügung gestellt. Dieses Dokument könnte als Orientierung dienen für:
- die Beurteilung der Qualität neuer Europäischer Normverfahren während ihrer Validierung;
- die Überprüfung der Qualität vorangegangener Laborvergleichsuntersuchungen;
- die Bestätigung der Erweiterung des Anwendungsbereichs einer bereits veröffentlichten Europäischen Norm, die für andere Analytkonzentrationen oder Matrices angewendet wurde; oder
- die Evaluierung der Gebrauchseignung einfach validierter Verfahren.
Die Leistungskriterien können auf Verfahren zur Bestimmung von Mykotoxinen anwendbar sein.

Aliments des animaux - Méthodes d'échantillonnage et d'analyse - Critères de performance des méthodes d'analyse des mycotoxines validées dans un seul laboratoire ou suite à un essai interlaboratoires

Le présent document spécifie les critères de performance pour la sélection de méthodes d’analyse des mycotoxines dans les aliments pour animaux validées dans un seul laboratoire ou suite à une étude collaborative. Il inclut les termes et définitions des paramètres pertinents pour la validation de la méthode. Il fournit également les exigences et caractéristiques de performance. Le présent document pourrait servir de guide :
— pour évaluer la qualité des nouvelles méthodes de Normes européennes en cours de validation ;
— pour examiner la qualité d’essais interlaboratoires antérieurs ;
— pour confirmer l’extension du domaine d’application d’une Norme européenne déj{ publiée, appliquée { d’autres concentrations d’analyte ou matrices ; ou
— pour évaluer l’adéquation { l’objectif de méthodes validées individuellement.
Les critères

Krma - Metode vzorčenja in analize - Izvedbena merila za validacijo metod v posameznem laboratoriju in v primerjalnem preskusu analiz za določanje mikotoksinov

General Information

Status
Published
Public Enquiry End Date
19-Dec-2019
Publication Date
18-Jun-2020
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
19-May-2020
Due Date
24-Jul-2020
Completion Date
19-Jun-2020

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17455:2020
01-julij-2020
Krma - Metode vzorčenja in analize - Izvedbena merila za validacijo metod v
posameznem laboratoriju in v primerjalnem preskusu analiz za določanje
mikotoksinov

Animal feeding stuffs - Methods of sampling and analysis - Performance criteria for

single laboratory validated and ring-trial validated methods of analysis for the
determination of mycotoxins
Futtermittel - Probenahme und Untersuchungsverfahren - Leistungskriterien für

laborintern validierte und im Ringversuch validierte Analysemethoden zur Bestimmung

von Mykotoxinen
Aliments des animaux - Méthodes d'échantillonnage et d'analyse - Critères de

performance des méthodes d'analyse des mycotoxines validées dans un seul laboratoire

ou suite à un essai interlaboratoires
Ta slovenski standard je istoveten z: CEN/TS 17455:2020
ICS:
65.120 Krmila Animal feeding stuffs
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST-TS CEN/TS 17455:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 17455:2020
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SIST-TS CEN/TS 17455:2020
CEN/TS 17455
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
April 2020
TECHNISCHE SPEZIFIKATION
ICS 65.120; 71.040; 71.040.50
English Version
Animal feeding stuffs - Methods of sampling and analysis -
Performance criteria for single laboratory validated and
ring-trial validated methods of analysis for the
determination of mycotoxins

Aliments des animaux - Méthodes d'échantillonnage et Futtermittel - Probenahme und

d'analyse - Critères de performance des méthodes Untersuchungsverfahren - Leistungskriterien für

d'analyse des mycotoxines validées dans un seul laborintern validierte und im Ringversuch validierte

laboratoire ou suite à un essai interlaboratoires Analysemethoden zur Bestimmung von Mykotoxinen

This Technical Specification (CEN/TS) was approved by CEN on 27 January 2020 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to

submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS

available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in

parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.

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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17455:2020 E

worldwide for CEN national Members.
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Contents Page

European foreword ....................................................................................................................................................... 3

Introduction ..................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 5

2 Normative references .................................................................................................................................... 5

3 Terms and definitions .................................................................................................................................... 5

4 Relation to other technical document definitions or concepts .................................................... 14

4.1 Reporting of sum parameters .................................................................................................................. 14

4.2 Requirements for multi-mycotoxin methods ..................................................................................... 14

4.3 Identification criteria .................................................................................................................................. 14

4.4 Limit of quantification (determination) and limit of detection ................................................... 14

5 Performance criteria for analytical methods for mycotoxins ...................................................... 15

5.1 General criteria for methods of analysis for mycotoxins ............................................................... 15

5.1.1 Overall concepts ............................................................................................................................................ 15

5.1.2 Screening methods for mycotoxins ........................................................................................................ 15

5.1.3 Confirmatory methods for mycotoxins ................................................................................................. 15

5.2 Performance characteristics .................................................................................................................... 16

5.2.1 General ............................................................................................................................................................. 16

5.2.2 Recovery .......................................................................................................................................................... 16

5.2.3 RSD .................................................................................................................................................................. 17

5.2.4 RSD ................................................................................................................................................................... 19

5.2.5 RSD ................................................................................................................................................................. 20

5.2.6 Limit of quantification ................................................................................................................................ 20

5.2.7 Minimum applicability range ................................................................................................................... 21

Bibliography ................................................................................................................................................................. 22

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European foreword

This document (CEN/TS 17455:2020) has been prepared by Technical Committee CEN/TC 327

“Animal feeding stuffs - Methods of sampling and analysis”, the secretariat of which is held by NEN.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document has been prepared under a mandate given to CEN by the European Commission and

the European Free Trade Association.

According to the CEN/CENELEC Internal Regulations, the national standards organisations of the

following countries are bound to announce this Technical Specification: 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,

Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and the United Kingdom.
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Introduction

The European Committee for Standardization (CEN) selects and elaborates methods of analysis for

organic contaminants that are to become European Standards. These standards can be used for those

contaminants that are subject to regulation. When used for this purpose, the main functions of a

standard are to enable feed manufacturers to determine with reasonable certainty whether a

consignment may be put on the market and to enable regulatory authorities to determine equitably

whether feedstuffs on the market comply with legal or recommended limits.

CEN/TC 327/working group (WG) 5 decided to establish a criteria guide in order to allow

benchmarking of methods of analysis for their fitness for purpose [1]. The performance criteria laid

down therein are based on published data, collected from official reports on inter-laboratory studies

[2] to [12].

Where performance characteristics are absent or limited in availability, the criteria were estimated

based on the experiences and opinions of the experts of the CEN working group. The selection criteria

could need updating in future revisions of this document, if newer or more accurate data on method

performance characteristics become available. This document lists relevant performance parameters

and gives information on their definition. It further describes how they can be practically obtained; it

indicates guidance values demonstrating fitness for purpose. As a result, these guidance values serve

as a benchmark for experienced analytical laboratories.

This document may contain useful information for CEN members, the European Commission, the

EFTA secretariat, other governmental agencies or outside bodies. The criteria in this CEN report are

used as guidance in the CEN/TC 327/WG 5. In general, method performance criteria are generated

for collaborative trials or for single laboratory validation (SLV) studies. The first case describes how a

method performs when used by several laboratories, giving greater confidence that the method is

applicable and can be implemented with the obtained method performance. The second case only

demonstrates how a method performs in a particular laboratory. As a result, SLV should be

conducted with care to avoid misinterpretation. This is important as reproducibility (between

laboratory variance) can only be derived from collaborative trials. Furthermore, performance

parameters such as limit of detection (LOD) and limit of quantification (LOQ) are laboratory specific

as the quantitative measurement capability strongly depends on the instrumental conditions used by

each laboratory.

This document relates to current EU legislation concerning performance requirements of analytical

methods for mycotoxins in food and feed chain, such as Regulation (EC) No 2017/625 on official

controls performed to ensure the verification of compliance with feed and food law, animal health

and animal welfare rules [13] as well as Regulation (EC) No 401/2006 laying down the methods of

sampling and analysis for the official control of the levels of mycotoxins in foodstuffs [14]. The latter

is specific for food, however as recent legislation on some mycotoxins does not specify the intended

final use, either food or feed, rather the raw commodity (Commission Recommendation

2013/165/EU on the presence of T-2 and HT-2 toxin in cereals and cereal products) performance

requirements for analytical methods are in the future anticipated to be equivalent independent of the

commodities' destination purpose.

Further this criteria approach document also relates to pre-existing documents such as the ISO 5725-

series, CR 13505 [15] and CEN/TR 16059 [16].
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1 Scope

This document specifies performance criteria for the selection of single-laboratory validated or

collaborative study validated methods of analysis of mycotoxins in feed. The terms and definition of

the relevant parameters for method validation are included. The performance requirements and

characteristics are provided. This document could serve as a guide:
— to assess the quality of new European Standard methods under validation;
— to review the quality of previous collaborative trials;

— to confirm the extension of the scope of an already published European Standard applied to

other analyte concentrations or matrices; or
— to evaluate the fitness-for-purpose of single-validated methods.

The performance criteria can apply to methods dedicated to the determination of mycotoxins.

2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp/ui
3.1
accuracy
closeness of agreement between a test result and the accepted reference value

Note 1 to entry: 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.
Note 2 to entry: It is assessed by determining trueness and precision.

[SOURCE: ISO 5725-1:1994, 3.6, see [17], modified; 2002/657/EEC, see [18], modified]

3.2
applicability

scope of the analytical method; description of the analytes, matrices, and concentration ranges (mass

fractions) for which a method of analysis can be used satisfactorily to determine compliance with a

given standard (i.e. CEN, ISO, CODEX)

Note 1 to entry: In addition to a statement of the range of capability of satisfactory performance for each

factor, the statement of applicability (scope) also includes warnings as to known interference by other analytes,

or inapplicability to certain matrices and situations.
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3.3
bias

difference between the expectation of the test results (x) and an accepted reference value (x )

ref

Note 1 to entry: The bias can be expressed in absolute or relative terms (b or b(%), respectively) as:

b xx−
(1)
ref
xx−
ref
b % ×100
( ) (2)
ref

[SOURCE: ISO 5725-1:1994, 3.8, see [17], modified; Eurachem 2014, see [19], modified]

3.4
inter-laboratory comparison

organisation, performance and evaluation of measurements or tests on the same or similar items by

two or more laboratories in accordance with predetermined conditions

Note 1 to entry: These conditions include that the materials have a suitable homogeneity and acceptable

stability that is documented.

Note 2 to entry: The larger the number of participating laboratories, the greater the confidence that can be

placed in the resulting statistical parameters.

Note 3 to entry: Vague terms such as “round-robins”, “intercalibrations”, “ring tests”, etc. should not be used.

Studies involving several laboratories with each preparing its own test materials and using its own methods,

are sometimes called cooperative studies.
[SOURCE: ISO/IEC 17043:2010, 3.4, see [20], modified]
3.4.1
collaborative study

inter-laboratory comparison aiming at the evaluation of the performance characteristics of a method

Note 1 to entry: It means analysing the same sample by the same method to determine the performance

characteristics of the method.
Note 2 to entry: The study covers random measurement error and laboratory bias.

Note 3 to entry: The reported results are used to estimate the performance characteristics of the method,

such as precision parameters like repeatability (within laboratory) and reproducibility (between laboratories).

When necessary and possible, other pertinent characteristics such as systematic error and/or recovery can be

reported. These can include bias, recovery, internal quality control parameters, sensitivity, limit of

quantification, and applicability.
[SOURCE: 2002/657/EEC, see [18], modified]
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3.4.2
proficiency testing

evaluation of participant performance against pre-established criteria by means of inter-laboratory

comparisons

Note 1 to entry: In practise the study consists of one or more analyses or measurements by a group of

laboratories on one or more homogeneous, stable test samples by the method selected or used by each

laboratory.

Note 2 to entry: The reported results are compared with those from other laboratories or with the known or

assigned reference value, usually with the objective of evaluating or improving laboratory performance.

Note 3 to entry: Proficiency testing means analysing the same sample allowing laboratories to choose their

own methods, provided these methods are used under routine conditions.

[SOURCE: 2002/657/EEC, see [18], modified; ISO/IEC 17043:2010, 3.7, see [20], modified]

3.4.3
reference material characterisation

inter-laboratory comparison aiming at the assignment of values to reference materials and

assessment of their suitability for use in specific test or measurement procedures

Note 1 to entry: The assigned values are usually the reference value (best estimate of the “true value”) to a

quantity (concentration/mass fraction) in the test material, usually with a stated uncertainty.

3.5
limit of detection
LOD

minimum amount or concentration of the analyte in a test sample which can be detected reliably but

not necessarily quantified, as demonstrated by a collaborative trial or other appropriate validation

Note 1 to entry: Guidelines for the sound generation of LOD values can be found in [23].

Note 2 to entry: 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 to entry: The various conceptual approaches to the subject depend on the estimate of precision at or

near zero concentration (mass fraction) under repeatability or reproducibility conditions.

[SOURCE: Thompson et al. 2002, see [21], modified; ISO 24276:2006, 3.1.6, see [22], modified]

3.6
limit of quantification
LOQ

lowest concentration or amount of the analyte in a test sample which can be quantitatively

determined with an acceptable level of precision and accuracy, as demonstrated by a collaborative

trial or other appropriate validation

Note 1 to entry: Rules for the sound generation of LOQ values can be found in [23].

Note 2 to entry: Measurements below LOQ are not void of information content. However, they are not of use

for method criteria assessment

[SOURCE: Thompson et al. 2002, see [21], modified; ISO 24276:2006, 3.1.7, see [22], modified]

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3.7
linearity

ability (within a given range) of an analytical procedure to obtain test results which are directly

proportional to the concentration (mass fraction) of analyte in the sample
[SOURCE: VAM/III/5626/94, see [24]]
3.8
lowest validated level

lowest concentration (mass fraction) investigated in the frame of a collaborative study or a single-

laboratory validation
3.9
precision

closeness of agreement between independent test results obtained under stipulated conditions

Note 1 to entry: 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 to entry: 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 to entry: “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.

[SOURCE: ISO 5725-1:1994, 3.12, see [17]]
3.9.1
repeatability
RSD
precision under repeatability conditions
[SOURCE: ISO 5725-1:1994, 3.13, see [17]]
3.9.1.1
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

[SOURCE: ISO 5725-1:1994, 3.14, see [17]]
3.9.1.2
repeatability standard deviation
standard deviation of test results obtained under repeatability conditions

Note 1 to entry: It is a measure of the dispersion of the distribution of test results under repeatability

conditions.

Note 2 to entry: Similarly “repeatability variance” and “repeatability coefficient of variation” could be defined

and used as measures of the dispersion of the test results under repeatability conditions.

[SOURCE: ISO 5725-1:1994, 3.15, see [17]]
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3.9.1.3
repeatability relative standard deviation
RSD

relative standard deviation of test results obtained under repeatability conditions

Note 1 to entry: The repeatability relative standard deviation (RSD ) can be expressed as follows:

RSD (%) × 100 (3)
mean
where:
c is the mean concentration (mass fraction).
mean
3.9.1.4
repeatability limit

value less than or equal to which the absolute difference between two test results obtained under

repeatability conditions may be expected to be within a probability of 95 %
Note 1 to entry: The repeatability limit (r) can be expressed as follows:
rs22× (4)
[SOURCE: ISO 5725-1:1994, 3.16, see [17]]
3.9.2
intermediate precision
precision under within-laboratory reproducibility conditions
3.9.2.1
within-laboratory reproducibility conditions

conditions where test results are obtained with the same method on identical test items on

different days with preferably different operators using different equipment
3.9.2.2
within-laboratory reproducibility standard deviation

standard deviation of test results obtained under within-laboratory reproducibility conditions

Note 1 to entry: It is a measure of the dispersion of the distribution of test results under within-laboratory

reproducibility conditions
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3.9.2.3
within-laboratory reproducibility relative standard deviation
RSD

relative standard deviation of test results obtained under within-laboratory reproducibility

conditions

Note 1 to entry: The within-laboratory reproducibility relative standard deviation (RSD ) can be expressed

as follows:
RSD % × 100
(5)
( )
mean
where

s is the standard deviation, calculated from results generated under within-laboratory

reproducibility conditions;
c is the mean concentration (mass fraction).
mean
3.9.3
reproducibility
precision under reproducibility conditions

Note 1 to entry: It is a measure of the dispersion of the distribution of test results under reproducibility

conditions.

Note 2 to entry: Equivalent terms used are “reproducibility variance” and “reproducibility coefficient of

variation” but should not be used in this context.
[SOURCE: ISO 5725-1:1994, 3.17, see [17], modified]
3.9.3.1
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
[SOURCE: ISO 5725-1:1994, 3.18, see [17]]
3.9.3.2
reproducibility standard deviation
standard deviation of test results obtained under reproducibility conditions

Note 1 to entry: It is a measure of the dispersion of the distribution of test results under reproducibility

conditions.

Note 2 to entry: 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.

[SOURCE: ISO 5725-1:1994, 3.19, see [17]]
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3.9.3.3
reproducibility relative standard deviation
RSD

relative standard deviation, calculated from results generated under reproducibility conditions

Note 1 to entry: The reproducibility relative standard deviation (RSD ) can be expressed as follows:

RSD (%) × 100 (6)
mean
where

s is the standard deviation, calculated from results generated under reproducibility conditions

c is the mean concentration (mass fraction).
mean
3.9.3.4
reproducibility limit

value less than or equal to which the absolute difference between two test results obtained under

reproducibility conditions may be expected to be within a probability of 95 %
Note 1 to entry: The reproducibility limit (R) can be expressed as follows:
R 22× s (7)
[SOURCE: ISO 5725-1:1994, 3.20, see [17], modified]
3.10
recovery
rec

percentage of the true concentration of a substance recovered during the analytical procedure

Note 1 to entry: An ideal approach to demonstrate that recovery is consistent over the whole working range

is to conduct a series of at least 4 fortification experiments over the whole working range. Linearity shall be

demonstrated by a “lack of fit” test. The slope of the curve is the recovery ( × 100 for expression in %), provided

the fortified increment mass fraction (c ) is plotted as X-axis against the measured mass fraction (c - c ) on the

+ f 0
Y-axis.

Note 2 to entry: Practical information for considerations in setting up recovery experiments are given in [25].

Note 3 to entry: The relative recovery (R ) can be expressed as:
rec
R (%) × 100
(8)
rec
ref
where:
x is the measured concentration (mass fraction);
x is the reference concentration (mass fraction)
ref
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Note 4 to entry: For fortified (spiked) samples, the relative recovery (R ) is the difference observed after

rec

analysis of the test material and fortified (spiked) to the test material and can be expressed as:

xx−
R (%) × 100 (9)
rec
spike
where:

x is the measured concentration (mass fraction) in the spiked or fortified sample;

x is the measured concentration (mass fraction) in the unfortified sample;
x is the spiked/added concentration (mass fraction).
spike

Note 5 to entry: Bias and recovery are correlated as follows: Recovery (%) + bias (%) = 100 %.

Note 6 to entry: The amount added for recovery estimation 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 7 to entry: A true or assigned value is known only in cases of 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.
[SOURCE: Eurachem Guide, see [19], modified]
3.11
ruggedness

resistance to changes in the results produced by an analytical method when minor deviations are

made from the experimental conditions described in the procedure

Note 1 to entry: It is the susceptibility of an analytical method to changes in experimental conditions which

can be expressed as a list of the sample materials, analytes, storage conditions, environmental and/or sample

preparation conditions under which the method can be applied as presented or with specified minor

modifications that are likely to occur during the analytical procedure.

Note 2 to entry: For all experimental conditions which could in practice be subject to fluctuation (e.g.

stability of reagents, composition of the sample, pH, temperature) any variations which could affect the

analytical result should be indicated.

Note 3 to entry: The term robustness is not recommended [24], as ruggedness is already been used by

Thompson et al. [21] and additional wording could lead to confusion.

[SOURCE: Thompson et al. 2002, see [21], modified; 2002/657/EEC, see [18], modified]

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3.12
selectivity

degree to which a method can quantify the analyte accurately in the presence of interferences

Note 1 to entry: For the determination and identification of mycotoxin the interferences are usually matrix

(feed material) derived components of similar physico-chemical behaviour, either exhibiting similar properties

during detection and/or separation such as sample clean-up or chromatographic separation.

Note 2 to entry: IUPAC recommends the us
...

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17455:2019
01-december-2019
Krma - Metode vzorčenja in analize - Izvedbena merila v posameznem laboratoriju
in v primerjalnem preskusu validirane metode analiz za določanje mikotoksinov

Animal feeding stuffs - Methods of sampling and analysis - Performance criteria for

single laboratory validated and ring-trial validated methods of analysis for the
determination of mycotoxins
Kriterienansatz für Methoden zur Analyse von Mycotoxinen in Futtermitteln
Aliments des animaux - Méthodes d’échantillonnage et d’analyse - Critères de

performance des méthodes d’analyse des mycotoxines validées dans un seul laboratoire

ou suite à un essai interlaboratoires
Ta slovenski standard je istoveten z: FprCEN/TS 17455
ICS:
65.120 Krmila Animal feeding stuffs
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
kSIST-TS FprCEN/TS 17455:2019 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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kSIST-TS FprCEN/TS 17455:2019
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17455
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
October 2019
ICS 65.120; 71.040; 71.040.50
English Version
Animal feeding stuffs - Methods of sampling and analysis -
Performance criteria for single laboratory validated and
ring-trial validated methods of analysis for the
determination of mycotoxins

Aliments des animaux - Méthodes d'échantillonnage et Kriterienansatz für Methoden zur Analyse von

d'analyse - Critères de performance des méthodes Mycotoxinen in Futtermitteln
d'analyse des mycotoxines validées dans un seul
laboratoire ou suite à un essai interlaboratoires

This draft Technical Specification is submitted to CEN members for Vote. It has been drawn up by the Technical Committee

CEN/TC 327.

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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

aware and to provide supporting documentation.

Warning : This document is not a Technical Specification. It is distributed for review and comments. It is subject to change

without notice and shall not be referred to as a Technical Specification.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TS 17455:2019 E

worldwide for CEN national Members.
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Contents Page

European foreword ....................................................................................................................................................... 3

Introduction ..................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 5

2 Normative references .................................................................................................................................... 5

3 Terms and definitions .................................................................................................................................... 5

4 Relation to other technical document definitions or concepts .................................................... 14

4.1 Reporting of sum parameters .................................................................................................................. 14

4.2 Requirements for multi-mycotoxin methods ..................................................................................... 14

4.3 Identification criteria .................................................................................................................................. 14

4.4 Limit of quantification (determination) and limit of detection ................................................... 14

5 Performance Criteria for analytical methods for mycotoxins ..................................................... 15

5.1 General Criteria for methods of analysis for mycotoxins .............................................................. 15

5.1.1 Overall concepts ............................................................................................................................................ 15

5.1.2 Screening methods for mycotoxins ........................................................................................................ 15

5.1.3 Confirmatory methods for mycotoxins ................................................................................................. 15

5.2 Performance characteristics .................................................................................................................... 16

5.2.1 General ............................................................................................................................................................. 16

5.2.2 Recovery .......................................................................................................................................................... 16

5.2.3 RSD .................................................................................................................................................................. 17

5.2.4 RSD ................................................................................................................................................................... 20

5.2.5 RSD ................................................................................................................................................................. 20

5.2.6 Limit of quantification ................................................................................................................................ 21

5.2.7 Minimum applicability range ................................................................................................................... 21

Bibliography ................................................................................................................................................................. 23

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European foreword

This document (FprCEN/TS 17455:2019) has been prepared by Technical Committee CEN/TC 327

“Animal feeding stuffs - Methods of sampling and analysis”, the secretariat of which is held by NEN.

This document is currently submitted to the Formal Vote.

This document has been prepared under a standardization request given to CEN by the European

Commission and the European Free Trade Association.
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Introduction

The European Committee for Standardization (CEN) selects and elaborates methods of analysis for

organic contaminants that are to become European Standards. These standards can be used for those

contaminants that are subject to regulation. When used for this purpose, the main functions of a

standard is to enable feed manufacturers to determine with reasonable certainty whether a

consignment may be put on the market and to enable regulatory authorities to determine equitably

whether feedstuffs on the market comply with legal or recommended limits.

CEN/TC 327/working group (WG) 5 decided to establish a criteria guide in order to allow

benchmarking of methods of analysis for their fitness for purpose [1]. The performance criteria laid

down therein are based on published data, collected from official reports on inter-laboratory studies

[2]-[12].

Where performance characteristics are absent or limited in availability, the criteria were estimated

based on the experiences and opinions of the experts of the CEN working group. The selection criteria

could need updating in future revisions of this document, if newer or more accurate data on method

performance characteristics become available. This document lists relevant performance parameters

and gives information on their definition. It further describes how they can be practically obtained; it

indicates guidance values demonstrating fitness for purpose. As a result, these guidance values can be

expected from (derived by) experienced analytical laboratories.

This document may contain useful information for CEN members, the European Commission, the

EFTA secretariat, other governmental agencies or outside bodies. The criteria in this CEN report are

used as guidance in the CEN/TC 327/WG 5. In general, method performance criteria are generated

for collaborative trials or for single laboratory validation studies. The first case describes how a

method performs when used by several laboratories, giving greater confidence that the method is

applicable and can be implemented with the obtained method performance. The second case only

demonstrates how a method performs in a particular laboratory. As a result, single laboratory

validation should be conducted with care to avoid misinterpretation. This is important as

reproducibility (between laboratory variance) can only be derived from collaborative trials.

Furthermore, performance parameters such as limit of detection (LOD) and limit of quantification

(LOQ) are laboratory specific as the quantitative measurement capability strongly depends on the

instrumental conditions used by each laboratory.

This document relates to current EU legislation concerning performance requirements of analytical

methods for mycotoxins in food and feed chain, such as Regulation (EC) No 2017/625 on official

controls performed to ensure the verification of compliance with feed and food law, animal health

and animal welfare rules [13] as well as Regulation (EC) No 401/2006 laying down the methods of

sampling and analysis for the official control of the levels of mycotoxins in foodstuffs [14]. The latter

is specific for food, however as recent legislation on some mycotoxins does not specify the intended

final use, either food or feed, rather the raw commodity (Commission Recommendation

2013/165/EU on the presence of T-2 and HT-2 toxin in cereals and cereal products) performance

requirements for analytical methods are in the future anticipated to be equivalent independent of the

commodities' destination purpose.

Further this criteria approach document also relates to pre-existing standards such as the ISO 5725-

series, CR 13505 [15] and CEN/TR 16059 [16].
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1 Scope

This document specifies performance criteria for the selection of single-laboratory validated or

collaborative study validated methods of analysis of mycotoxins in feed. The terms and definition of

the relevant parameters for method validation are included. The performance requirements and

characteristics are provided. This document could serve as a guide:
— to assess the quality of new European Standard methods under validation;
— to review the quality of previous collaborative trials;

— to confirm the extension of the scope of an already published European Standard applied to

other analyte concentrations or matrices; or
— to evaluate the fitness-for-purpose of single-validated methods.

The performance criteria can apply to methods dedicated to the determination of mycotoxins.

2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
3.1
accuracy
closeness of agreement between a test result and the accepted reference value

Note 1 to entry: 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.
Note 2 to entry: It is assessed by determining trueness and precision.

[SOURCE: ISO 5725-1:1994, 3.6, see [17], modified; 2002/657/EEC, see [18]modified]

3.2
applicability

scope of the analytical method; description of the analytes, matrices, and concentration ranges (mass

fractions) for which a method of analysis can be used satisfactorily to determine compliance with a

given standard (i.e. CEN, ISO, CODEX)

Note 1 to entry: In addition to a statement of the range of capability of satisfactory performance for each

factor, the statement of applicability (scope) also includes warnings as to known interference by other analytes,

or inapplicability to certain matrices and situations.
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3.3
bias

difference between the expectation of the test results (x) and an accepted reference value (x )

ref

Note 1 to entry: The bias can be expressed in absolute or relative terms (b or b(%), respectively) as:

b xx−
(1)
ref
xx−
ref
b % ×100 (2)
( )
ref

[SOURCE: ISO 5725-1:1994, 3.8, see [17], modified; Eurachem 2014, see [19], modified]

3.4
inter-laboratory comparison

organisation, performance and evaluation of measurements or tests on the same or similar items by

two or more laboratories in accordance with predetermined conditions

Note 1 to entry: These conditions include that the materials have a suitable homogeneity and acceptable

stability that is documented.

Note 2 to entry: The larger the number of participating laboratories, the greater the confidence that can be

placed in the resulting statistical parameters.

Note 3 to entry: Vague terms such as “round-robins”, “intercalibrations”, “ring tests”, etc. should not be used.

Studies involving several laboratories with each preparing its own test materials and using its own methods,

are sometimes called cooperative studies.
[SOURCE: ISO/IEC 17043:2010, 3.4, see [20], modified]
3.4.1
collaborative study

inter-laboratory comparison aiming at the evaluation of the performance characteristics of a method

Note 1 to entry It means analysing the same sample by the same method to determine the performance

characteristics of the method.
Note 2 to entry The study covers random measurement error and laboratory bias.

Note 3 to entry: The reported results are used to estimate the performance characteristics of the method,

such as precision parameters like repeatability (within laboratory) and reproducibility (between laboratories).

When necessary and possible, other pertinent characteristics such as systematic error and/or recovery can be

reported. These can include bias, recovery, internal quality control parameters, sensitivity, limit of

quantification, and applicability.
[SOURCE: 2002/657/EEC, see [18], modified]
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3.4.2
proficiency testing

evaluation of participant performance against pre-established criteria by means of inter-laboratory

comparisons

Note 1 to entry: In practise the study consists of one or more analyses or measurements by a group of

laboratories on one or more homogeneous, stable test samples by the method selected or used by each

laboratory.

Note 2 to entry: The reported results are compared with those from other laboratories or with the known or

assigned reference value, usually with the objective of evaluating or improving laboratory performance.

Note 3 to entry Proficiency testing means analysing the same sample allowing laboratories to choose their

own methods, provided these methods are used under routine conditions.

[SOURCE: 2002/657/EEC, see [18], modified; ISO/IEC 17043:2010, 3.7, see [20], modified]

3.4.3
reference material characterisation

inter-laboratory comparison aiming at the assignment of values to reference materials and

assessment of their suitability for use in specific test or measurement procedures

Note 1 to entry: The assigned values are usually the reference value (best estimate of the “true value”) to a

quantity (concentration/mass fraction) in the test material, usually with a stated uncertainty.

3.5
limit of detection
LOD

minimum amount or concentration of the analyte in a test sample which can be detected reliably but

not necessarily quantified, as demonstrated by a collaborative trial or other appropriate validation

Note 1 to entry: Guidelines for the sound generation of LOD values can be found in [23].

Note 2 to entry: 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 to entry: The various conceptual approaches to the subject depend on the estimate of precision at or

near zero concentration (mass fraction) under repeatability or reproducibility conditions.

[SOURCE: Thompson et al. 2002, see [21], modified; ISO 24276:2006, 3.1.6, see [22], modified]

3.6
limit of quantification
LOQ

lowest concentration or amount of the analyte in a test sample which can be quantitatively

determined with an acceptable level of precision and accuracy, as demonstrated by a collaborative

trial or other appropriate validation

Note 1 to entry: Rules for the sound generation of LOQ values can be found in [23].

Note 2 to entry: Measurements below LOQ are not void of information content. However, they are not of use

for method criteria assessment

[SOURCE: Thompson et al. 2002, see [21], modified; ISO 24276:2006, 3.1.7, see [22], modified]

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3.7
linearity

ability (within a given range) of an analytical procedure to obtain test results which are directly

proportional to the concentration (mass fraction) of analyte in the sample
[SOURCE: VAM/III/5626/94, see [24]]
3.8
lowest validated level

lowest concentration (mass fraction) investigated in the frame of a collaborative study or a single-

laboratory validation
3.9
precision

closeness of agreement between independent test results obtained under stipulated conditions

Note 1 to entry: 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 to entry: 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 to entry: “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.

[SOURCE: ISO 5725-1:1994, 3.12, see [17]]
3.9.1
repeatability
RSD
precision under repeatability conditions
[SOURCE: ISO 5725-1:1994, 3.13, see [17]]
3.9.1.1
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

[SOURCE: ISO 5725-1:1994, 3.14, see [17]]
3.9.1.2
repeatability standard deviation
standard deviation of test results obtained under repeatability conditions

Note 1 to entry: It is a measure of the dispersion of the distribution of test results under repeatability

conditions.

Note 2 to entry: Similarly “repeatability variance” and “repeatability coefficient of variation” could be defined

and used as measures of the dispersion of the test results under repeatability conditions.

[SOURCE: ISO 5725-1:1994, 3.15, see [17]]
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3.9.1.3
repeatability relative standard deviation
RSD

relative standard deviation of test results obtained under repeatability conditions

Note 1 to entry: The repeatability relative standard deviation (RSD ) can be expressed as follows:

RSD (%) × 100 (4)
mean
where:
c is the mean concentration (mass fraction).
mean
3.9.1.4
repeatability limit

value less than or equal to which the absolute difference between two test results obtained under

repeatability conditions may be expected to be within a probability of 95 %
Note 1 to entry: The repeatability limit (r) can be expressed as follows:
rs22× (5)
[SOURCE: ISO 5725-1:1994, 3.16, see [17]]
3.9.2
intermediate precision
precision under within-laboratory reproducibility conditions
3.9.2.1
within-laboratory reproducibility conditions

conditions where test results are obtained with the same method on identical test items on different

days with preferably different operators using different equipment
3.9.2.2
within-laboratory reproducibility standard deviation

standard deviation of test results obtained under within-laboratory reproducibility conditions

Note 1 to entry: It is a measure of the dispersion of the distribution of test results under within-laboratory

reproducibility conditions
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3.9.2.3
within-laboratory reproducibility relative standard deviation
RSD

relative standard deviation of test results obtained under within-laboratory reproducibility

conditions

Note 1 to entry: The within-laboratory reproducibility relative standard deviation (RSD ) can be expressed

as follows:
RSD % × 100
(6)
( )
mean
where

s is the standard deviation, calculated from results generated under within-laboratory

reproducibility conditions;
c is the mean concentration (mass fraction).
mean
3.9.3
reproducibility
precision under reproducibility conditions

Note 1 to entry: It is a measure of the dispersion of the distribution of test results under reproducibility

conditions.

Note 2 to entry: Equivalent terms used are “reproducibility variance” and “reproducibility coefficient of

variation” but should not be used in this context.
[SOURCE: ISO 5725-1:1994, 3.17, see [17], modified]
3.9.3.1
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
[SOURCE: ISO 5725-1:1994, 3.18, see [17]]
3.9.3.2
reproducibility standard deviation
standard deviation of test results obtained under reproducibility conditions

Note 1 to entry: It is a measure of the dispersion of the distribution of test results under reproducibility

conditions.

Note 2 to entry: 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.

[SOURCE: ISO 5725-1:1994, 3.19, see [17]]
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3.9.3.3
reproducibility relative standard deviation
RSD

relative standard deviation, calculated from results generated under reproducibility conditions

Note 1 to entry: The reproducibility relative standard deviation (RSD ) can be expressed as follows:

RSD (%) × 100 (7)
mean
where

S is the standard deviation, calculated from results generated under reproducibility conditions

c is the mean concentration (mass fraction).
mean
3.9.3.4
reproducibility limit

value less than or equal to which the absolute difference between two test results obtained under

reproducibility conditions may be expected to be within a probability of 95 %
Note 1 to entry: The reproducibility limit (R) can be expressed as follows:
R 22× s
(8)
[SOURCE: ISO 5725-1:1994, 3.20, see [17], modifed]
3.10
recovery
rec

percentage of the true concentration of a substance recovered during the analytical procedure

Note 1 to entry: An ideal approach to demonstrate that recovery is consistent over the whole working range

is to conduct a series at least 4 fortification experiments over the whole working range. Linearity shall be

demonstrated by a “lack of fit” test. The slope of the curve for recovery determination ( × 100 for expression in

%), provided the fortified increment mass fraction (c ) is plotted as X-axis against the measured mass fraction

(c - c ) on the Y-axis.
f 0

Note 2 to entry: Practical information for considerations in setting up recovery experiments are given in [25].

Note 3 to entry: The relative recovery (R ) can be expressed as:
rec
R (%) × 100
(9)
rec
ref
where:
x is the measured concentration (mass fraction);
x is the reference concentration (mass fraction)
ref
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Note 4 to entry: For fortified (spiked) samples, the relative recovery (R ) is the difference observed after

rec

analysis of the test material and fortified (spiked) to the test material and can be expressed as:

xx−
R (%) × 100 (10)
rec
spike
where:

x is the measured concentration (mass fraction) in the spiked or fortified sample;

x is the measured concentration (mass fraction) in the unfortified sample;
x is the spiked/added concentration (mass fraction).
spike

Note 5 to entry: Bias and recovery are correlated as follows: Recovery (%) + bias (%) = 100 %.

Note 6 to entry: The amount added for recovery estimation 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 7 to entry: A true or assigned value is known only in cases of 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.
[SOURCE: EuraChem Guide, see [19], modified]
3.11
ruggedness

resistance to changes in the results produced by an analytical method when minor deviations are

made from the experimental conditions described in the procedure

Note 1 to entry: It is the susceptibility of an analytical method to changes in experimental conditions which

can be expressed as a list of the sample materials, analytes, storage conditions, environmental and/or sample

preparation conditions under which the method can be applied as presented or with specified minor

modifications that are likely to occur during the analytical procedure.

Note 2 to entry: For all experimental conditions which could in practice be subject to fluctuation (e.g.

stability of reagents, composition of the sample, pH, temperature) any variations which could affect the

analytical result should be indicated.

Note 3 to entry: The term robustness is not recommended [24], as ruggedness is already been used by

Thomason et al. [21] and additional wording could lead to confusion.

[SOURCE: Thompson et al. 2002, see [21], modified; 2002/657/EEC, see [18], modified]

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3.12
selectivity

degree to which a method can quantify the analyte accurately in the presence of interferences

Note 1 to entry: For the determination and identification of mycotoxin the interferences are usually matrix

(feed material) derived components of similar physico-chemical behaviour, either exhibiting similar properties

during detection and/or separation such as sample clean-up or chromatographic separation.

Note 2 to entry: IUPAC recommends the use of the term “selectivity” and discourages the use of the term

“specificity”. IUPAC clarified this overlap by expressing the view that “Specificity is the ultimate of Selectivity”

Note 3 to entry: Ideally, selectivity should be evaluated for any important interferences likely to be present.

It is particularly important to check interferences that are likely, on physico-chemical principles, to respond to

the test. As a general principle, selectivity should be sufficiently good for any interferences to be ignored.

[SOURCE: Thompson et al. 2002, see [21], modified; Wessmann et al. 2001, see [26], modifed]

3.13
sensitivity
gradient or slope of the calibration function of a method

Note 1 to entry: As this is usually arbitrary, depending on instrumental settings, it is not useful in validation.

It could be useful in quality assurance procedures, however, to test whether an instrument is performing to a

...

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