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