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BS EN 12393-2:2013

$189.07

Foods of plant origin. Multiresidue methods for the determination of pesticide residues by GC or LC-MS/MS – Methods for extraction and clean-up

Published By Publication Date Number of Pages
BSI 2013 46
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This European Standard specifies methods for the extraction and clean-up of food samples of plant origin for quantitative determination of pesticide residues.

Different solvents can be used for this purpose. These pesticide residues are generally associated with other co-extracted compounds which would interfere in the analysis. To purify the crude extracts to be analysed, several techniques can be used.

This European Standard contains the following extraction and clean-up methods that have been subjected to interlaboratory studies and/or are adopted throughout Europe:

  • method M: Extraction with acetone and liquid-liquid partition with dichloromethane/light petroleum, if necessary clean-up on Florisil® 1) [1], [2], [3];

  • method N: Extraction with acetone, liquid-liquid partition with dichloromethane or cyclohexane/ethyl acetate and clean-up with gel permeation and silica gel chromatography [4], [5];

  • method P: Extraction with ethyl acetate, and if necessary, clean-up by gel permeation chromatography [6].

This European Standard specifies the details of methods M, N and P for the extraction and the clean-up of food samples of plant origin. Several solvents at different volumes are used for extraction. Techniques of clean-up are listed such as liquid-liquid partition, liquid chromatography on various adsorbents and gel permeation chromatography.

A table providing the couples (matrix/pesticide) which have been submitted to collaborative studies and a list of indicative applicability of the method to different pesticides are given for each method, wherever possible.

PDF Catalog

PDF Pages PDF Title
4 Contents Page
5 Foreword
6 Introduction
7 1 Scope
2 Normative references
3 Principles
8 4 General: Summary of procedures
4.1 Extraction
4.2 Clean-up
4.2.1 Liquid-liquid partition
4.2.2 Adsorption column chromatography
4.2.3 Gel permeation chromatography with Bio-Beads® S-X31F )
9 5 Method M: Extraction with acetone and liquid-liquid partition with dichloromethane/light petroleum, if necessary clean-up on Florisil®
5.1 Principle
5.2 Reagents
10 5.3 Apparatus
5.4 Procedure
5.4.1 Preparation of the sample
5.4.2 Extraction and partition
5.4.3 Clean-up
5.4.3.1 Method M1
11 5.4.3.2 Method M2
5.5 Gas chromatography
5.6 Calculation of residues
12 6 Method N: Extraction with acetone, liquid-liquid partition with dichloromethane or cyclohexane/ethyl acetate, clean-up with gel permeation and silica gel chromatography
6.1 Principle
6.2 Reagents
13 6.3 Apparatus
14 6.4 Procedure
6.4.1 Extraction
6.4.1.1 General
6.4.1.2 Plant material and other foods with a water content exceeding 70 g/100 g
6.4.1.3 Plant material with low water content
6.4.2 Partition
6.4.2.1 Partition with dichloromethane
15 6.4.2.2 Partition with cyclohexane/ethyl acetate
6.4.3 Clean-up by gel permeation chromatography
6.4.3.1 General
6.4.3.2 Packing gel permeation column
6.4.3.3 Checking elution volumes
6.4.3.4 Clean-up of crude extracts
16 6.4.4 Additional clean-up for GC determination: Chromatography on a silica gel minicolumn
6.4.4.1 Preparation of column
6.4.4.2 Checking separation efficiency of silica gel
6.4.4.3 Fractionation of sample extract
27 6.5 Gas chromatography
28 6.6 Liquid chromatography with tandem-mass spectrometric detection (LC-MS/MS)
6.7 Calculation of residues
29 6.8 Collaborative studies
36 6.9 Applicability
37 7 Method P: Extraction with ethyl acetate, and if necessary, clean-up by gel permeation chromatography
7.1 Principle
7.2 Reagents
7.3 Apparatus
38 7.4 Procedure
7.4.1 Preparation of the sample
7.4.2 Extraction
7.4.3 Clean-up by gel permeation chromatography (if required)
7.4.3.1 Packing gel permeation column
7.4.3.2 Checking elution volumes
39 7.4.3.3 Clean-up of crude extracts
7.5 Gas chromatography
7.6 Liquid chromatography
7.7 Calculation of results
40 7.8 Proficiency testing data
7.9 Applicability
43 Annex A (informative) Average water content of crops and foods
44 Bibliography
BS EN 12393-2:2013
$189.07