Modification and re-validation of the ethyl acetate-based multi-residue method for pesticides in produce |
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Authors: | Hans G J Mol Astrid Rooseboom Ruud van Dam Marleen Roding Karin Arondeus Suryati Sunarto |
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Institution: | (1) Rikilt Institute of Food Safety, Pesticides and Contaminants, P.O. Box 230, 6700 AE Wageningen, The Netherlands;(2) TNO-Blgg-AgriQ, P.O. Box 392, 6700 AJ Wageningen, The Netherlands;(3) Department Analytical Research, TNO Quality of Life, P.O. Box 513, 3700 AJ Zeist, The Netherlands |
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Abstract: | The ethyl acetate-based multi-residue method for determination of pesticide residues in produce has been modified for gas
chromatographic (GC) analysis by implementation of dispersive solid-phase extraction (using primary–secondary amine and graphitized
carbon black) and large-volume (20 μL) injection. The same extract, before clean-up and after a change of solvent, was also
analyzed by liquid chromatography with tandem mass spectrometry (LC–MS–MS). All aspects related to sample preparation were
re-assessed with regard to ease and speed of the analysis. The principle of the extraction procedure (solvent, salt) was not
changed, to avoid the possibility invalidating data acquired over past decades. The modifications were made with techniques
currently commonly applied in routine laboratories, GC–MS and LC–MS–MS, in mind. The modified method enables processing (from
homogenization until final extracts for both GC and LC) of 30 samples per eight hours per person. Limits of quantification
(LOQs) of 0.01 mg kg−1 were achieved with both GC–MS (full-scan acquisition, 10 mg matrix equivalent injected) and LC–MS–MS (2 mg injected) for
most of the pesticides. Validation data for 341 pesticides and degradation products are presented. A compilation of analytical
quality-control data for pesticides routinely analyzed by GC–MS (135 compounds) and LC–MS–MS (136 compounds) in over 100 different
matrices, obtained over a period of 15 months, are also presented and discussed. At the 0.05 mg kg−1 level acceptable recoveries were obtained for 93% (GC–MS) and 92% (LC–MS–MS) of pesticide–matrix combinations. |
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Keywords: | Foods/Beverages Pesticides GC-MS LC-MS/MS Multi-residue analysis |
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