Title
Modification and re-validation of the ethyl acetate-based multi-residue method for pesticides in produce
Author
Mol, H.G.J.
Rooseboom, A.
van Dam, R.
Roding, M.
Arondeus, K.
Sunarto, S.
TNO Kwaliteit van Leven
Publication year
2007
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. © 2007 Springer-Verlag.
Subject
Agriculture Chemistry
Analytical research
Foods/Beverages
GC-MS
LC-MS/MS
Multi-residue analysis
Pesticides
Amines
Carbon black
Degradation
Extraction
Fruits
Gas chromatography
Liquid chromatography
Mass spectrometry
Ethyl acetate
Limits of quantification
Multi-residue analysis
Solid phase extraction
Pesticides
acetic acid derivative
acetic acid ethyl ester
amine
carbon
pesticide residue
article
chemistry
food contamination
gas chromatography
liquid chromatography
methodology
plant
reproducibility
sensitivity and specificity
solid phase extraction
tandem mass spectrometry
Acetates
Amines
Carbon
Chromatography, Gas
Chromatography, Liquid
Food Contamination
Pesticide Residues
Plants, Edible
Reproducibility of Results
Sensitivity and Specificity
Solid Phase Extraction
Tandem Mass Spectrometry
To reference this document use:
http://resolver.tudelft.nl/uuid:7964dcb1-8306-4057-b047-e0b6f9a35cdb
DOI
https://doi.org/10.1007/s00216-007-1357-1
TNO identifier
240284
ISSN
1618-2642
Source
Analytical and Bioanalytical Chemistry, 389 (6), 1715-1754
Document type
article