CEN/TS 17061:2017

SLOVENSKI STANDARD
01-november-2017
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Foodstuffs - Guidelines for the calibration and quantitative determination of pesticide
residues and organic contaminants using chromatographic methods
Lebensmittel - Leitfaden für die Kalibrierung und die Auswertung von
Analysenergebnissen bei der Anwendung chromatographischer Methoden für die
quantitative Bestimmung von Pflanzenschutzmittelrückständen und organischen
Kontaminanten
Produits alimentaires - Lignes directrices pour l’étalonnage et le dosage des résidus de
pesticides et contaminants organiques par des méthodes chromatographiques
Ta slovenski standard je istoveten z: CEN/TS 17061:2017
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

CEN/TS 17061
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
September 2017
TECHNISCHE SPEZIFIKATION
ICS 67.050
English Version
Foodstuffs - Guidelines for the calibration and quantitative
determination of pesticide residues and organic
contaminants using chromatographic methods
Produits alimentaires - Lignes directrices pour Lebensmittel - Leitfaden für die Kalibrierung und die
l'étalonnage et le dosage des résidus de pesticides et Auswertung von Analysenergebnissen bei der
contaminants organiques par des méthodes Anwendung chromatographischer Methoden für die
chromatographiques quantitative Bestimmung von
Pflanzenschutzmittelrückständen und organischen
Kontaminanten
This Technical Specification (CEN/TS) was approved by CEN on 11 May 2017 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, 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: Avenue Marnix 17, B-1000 Brussels
© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17061:2017 E
worldwide for CEN national Members.

Contents Page
European foreword . 4
1 Scope . 5
2 Principle . 5
3 General . 5
4 Execution and calculation of calibrations . 6
4.1 General/specifications . 6
4.1.1 Working range. 6
4.1.2 Number of calibration points . 6
4.1.3 Permissible quantities for determination of response (peak areas or peak heights
and peak ratio, respectively) . 7
4.1.4 Stability of calibration functions . 8
4.2 Calibration functions . 8
4.2.1 Selection of appropriate calibration function . 8
4.2.2 Visual linearity test . 8
4.2.3 Mathematical check of linearity . 9
4.2.4 Calibration with interpolation functions. 9
4.3 Test for matrix effects . 10
4.4 Basic calibration and calibration by means of external standard. 10
4.4.1 Basic calibration . 10
4.4.2 Calculation by means of external standard in case of linear calibration function
without significant ordinate intercept . 10
4.4.3 Calculation by means of external standard using linear calibration function. 11
4.4.4 Calculation by means of external standard using quadratic calibration function . 11
4.4.5 Calculation by means of external standard using nonlinear calibration function or
weighted regression . 12
4.5 Calculation by means of internal standard . 12
4.5.1 General . 12
4.5.2 Calculation with internal correction standard . 13
4.5.3 Calculation with stable-isotope labelled standard . 14
4.6 Calibration using standard addition procedures . 16
4.6.1 General . 16
4.6.2 Standard addition to the final extract. 16
4.6.3 Standard addition to the sample before extraction . 17
4.7 Procedural calibration . 18
4.8 Calibration with chemical conversion of the standard . 18
5 Quality assurance . 18
5.1 Qualification of the chromatographic system . 18
5.1.1 Equipment qualification . 18
5.1.2 Drift of a calibration system . 19
5.1.3 Performance criteria for GC and HPLC measurements . 19
5.2 Examination of integration results . 19
5.3 Permissible blank values in relation to the lower limit of working range . 19
5.4 Frequency of calibrations . 20
5.5 Number of analytes to be calibrated for “multi-methods” . 20
5.6 Handling of substances with multiple peaks . 20
5.7 Quality control chart . 20
6 Expression of results (units, number of significant figures). 22
7 Examples . 23
7.1 Example 1 — Test for variance inhomogeneity . 23
7.2 Example 2 — Selection of appropriate calibration function . 23
7.3 Example 3 — Test for matrix effects . 30
7.4 Example 4 — Calibration with external standard . 31
7.5 Example 5 — Calibration with internal standard . 33
7.6 Example 6 — Calculation with stable-isotope labelled standard . 34
7.7 Example 7 — Standard addition to final extract . 35
Bibliography . 37

European foreword
This document (CEN/TS 17061:2017) 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 shall not be held responsible for identifying any or all such patent rights.
Annex A (informative) contains a list of abbreviations.
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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
1 Scope
This Technical Specification describes the execution of calibration and quantitative evaluation of
chromatographic procedures for the determination of pesticides and organic contaminants in residue
analysis. In addition, the essential requirements for calibration are outlined.
The calibration of analytical procedures and the evaluation of analytical results need to be conducted
according to uniform principles in order to allow for a comparison of analytical results (even from
different analytical procedures). They constitute the basis of any method validation and of the quality
assurance within laboratories [1], [2], [3].
This Technical Specification does not consider issues of identification/qualification and extraction
efficiency.
2 Principle
This document describes the approach for the calibration of chromatographic procedures. The
following types of calibration are discussed in more detail:
— external calibration with linear calibration function;
— external calibration with quadratic calibration function;
— calibration with internal standard and linear calibration function;
— calibration with internal standard and quadratic calibration function;
— calibration with standards labelled with stable isotopes (isotopic dilution analysis);
— standard addition to final extract;
— standard addition to sample.
For this purpose, the calibration function and the selection criteria are illustrated on the basis of
examples. The calculation formulae refer to the final extract ready for analysis (“test solution”).
The description is rounded off by essential items of quality assurance, e.g. the qualification of
chromatographic systems or the quality control chart.
3 General
Calibration of a system is understood as the determination of a functional relationship between a
measurable quantity and a concentration to be determined. The chosen type of calibration depends on
the various analytical problems/tasks. It is performed in connection with the respective series of
measurements.
Basic ca
...