EN 12393-3:2013

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Pflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrückständen mit GC oder LC-MS/MS - Teil 3: Verfahren zur Bestimmung und AbsicherungAliments d'origine végétale - Méthodes multirésidus de détermination de résidus de pesticides par CPG ou CL-SM/SM - Partie 3: Détermination et essais de confirmationFoods of plant origin - Multiresidue methods for the determination of pesticide residues by GC or LC-MS/MS - Part 3: Determination and confirmatory tests67.080.01Sadje, zelenjava in njuni proizvodi na splošnoFruits, vegetables and derived products in general67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 12393-3:2013SIST EN 12393-3:2014en,fr,de01-januar-2014SIST EN 12393-3:2014SLOVENSKI
STANDARDSIST EN 12393-3:20091DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 12393-3
November 2013 ICS 67.050 Supersedes EN 12393-3:2008English Version
Foods of plant origin - Multiresidue methods for the determination of pesticide residues by GC or LC-MS/MS - Part 3: Determination and confirmatory tests
Aliments d'origine végétale - Méthodes multirésidus de détermination de résidus de pesticides par CPG ou CL-SM/SM - Partie 3: Détermination et essais de confirmation Pflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrückständen mit GC oder LC-MS/MS - Teil 3: Verfahren zur Bestimmung und Absicherung This European Standard was approved by CEN on 21 September 2013.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.
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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
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Typical GC operating conditions . 10 Annex B (informative)
Typical GC-MS/MS-operating conditions . 12 Annex C (informative)
Typical LC operating conditions . 16 Bibliography . 20
4.1.1 Identification A number of parameters can be employed to determine the identity of an analyte present in the sample extract. This includes:
a) retention time of the analyte in question (RT) or, even better, the retention time ratio against the ISTD (Rt(A)/Rt(ISTD)) obtained from the same run (the simultaneous use of columns of different polarity improves this type of identification);
b) in case of MS or MS/MS detection, the relative abundance of simultaneously recorded signals (in general 3 ions are required in MS applications and 2 SRM transitions in MS/MS);
c) the application of high resolution mass spectrometry;
d) in case of MS with electron impact ionisation the comparison of the full scan mass spectrum of a suspected peak (when indicated after subtraction of background) with spectral libraries; SIST EN 12393-3:2014

For more information about the required identification criteria, see [1]. 4.1.2 Quantification For quantification, a chromatographic system calibrated with an sufficient number of appropriately distributed calibration points has to be used. The precision of calibration has to fulfil minimum requirements. Make sure that all the measurements are performed within the calibrated range of the system. In exceptional cases only, single-level calibration may be used. It has to be checked that the response of analytes present in complex mixtures does not differ from the response of separate analytes. Mixtures of isomers, degradation products and derivatives of analytes may require special conditions during calibration. For calibration, either standards in solvents or standards prepared in blank matrix (matrix-matched standards) may be used. If matrix effects during GC injection or atmospheric pressure ionisation cannot be excluded, the use of matrix-matched standards or, even better, a quantification by standard addition has to be preferred. To detect instable detector response or such errors, which influence the amount of the analyte in the final extract, one or more internal standards should be added either to extracts or before extraction. To consider specific losses of individual analytes or their matrix effects, stable isotope labelled standards (if available) may be added to the sample before extraction.
All signals automatically identified by software tools may be considered as potential pesticide residues. However, any final quantification of relevant pesticide residues should be based on visual inspection of chromatograms. Before this European Standard can be used to quantify pesticides which are not tested before, a complete initial method validation is required. In all other cases, an on-going performance verification is sufficient to demonstrate the accuracy of the analytical method in a given laboratory.
For more information about the required quantification criteria, see [1] in its current version. 4.2 Gas chromatography (GC) 4.2.1 General The detectors (see EN 12393-1:2013, 3.4) should be properly adjusted, according to the manufacturers' instructions. Variations in detector sensitivity should be checked periodically by verifying the linearity of the calibration curves using standard solutions of pesticides. The measurement may be performed using various instruments, instrument parameters and columns. Some suitable instrument parameters and columns are listed in Annexes A and B.
For suitable experimental conditions of GC-MS measurement, see [2]. For suitable experimental conditions of GC-MS/MS measurement, see [3]. It has been found in practice that equivalent results can be achieved despite the adoption of different GC conditions, and different vendors of instruments. On the other hand, specifying standard GC parameters does not guarantee that the quality of the results generated will be identical. SIST EN 12393-3:2014
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