PMID- 18343389 OWN - NLM STAT- MEDLINE DCOM- 20080924 LR - 20240109 IS - 0021-9673 (Print) IS - 0021-9673 (Linking) VI - 1196-1197 DP - 2008 Jul 4 TI - Determination of 23 pesticide residues in leafy vegetables using gas chromatography-ion trap mass spectrometry and analyte protectants. PG - 100-9 LID - 10.1016/j.chroma.2008.02.087 [doi] AB - A gas chromatographic method was developed for simultaneously determining residues of 12 insecticides (acrinathrin, bifenthrin, carbofuran, cyfluthrin, lambda-cyhalothrin, cypermethrin, chlorfenvinphos, deltamethrin, esfenvalerate, fenamiphos, methiocarb and tau-fluvalinate) and 11 fungicides (cyprodinil, fludioxonil, iprodione, metalaxyl, penconazole, pyrimethanil, procymidone tebuconazole, triadimefon, triadimenol and vinclozolin) in leafy vegetables. Samples were extracted with acetonitrile and cleaned-up with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. The eluate was finally evaporated and redissolved with 0.5 mL of acetone containing the internal standards (pentachlorobenzene and fenpropathrin) and three analyte protectants (3-ethoxy-1,2-propanediol, d-sorbitol and l-gulonic acid gamma-lactone). The addition of analyte protectants allows to avoid the matrix-induced response enhancement effect on quantitation process with absolute recoveries ca. 100%. Precision (expressed as relative standard deviation) was lower than 10% for all pesticides and finally, limits of detection were also 10-20 times lower than maxima residue levels (MRLs) established by European Regulation. The proposed method was applied to determine pesticide residues in commercial leafy vegetables (lettuce, Swiss chard and spinach) purchased from markets in Orense (NW Spain). Pesticide residues were detected in 84% of the total samples (63 from 75 samples) and pesticide concentrations were higher than MRL in 18 samples. FAU - Gonzalez-Rodriguez, Rosa Ma AU - Gonzalez-Rodriguez RM AD - Nutrition and Bromatology Group, Analytical and Food Chemistry Department, Faculty of Food Science and Technology, University of Vigo, Ourense Campus, Ourense, Spain. FAU - Rial-Otero, Raquel AU - Rial-Otero R FAU - Cancho-Grande, Beatriz AU - Cancho-Grande B FAU - Simal-Gandara, Jesus AU - Simal-Gandara J LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20080302 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Pesticide Residues) SB - IM MH - Gas Chromatography-Mass Spectrometry/*methods MH - Molecular Structure MH - Pesticide Residues/*analysis/chemistry/isolation & purification MH - Plant Leaves/*chemistry MH - Reference Standards MH - Reproducibility of Results MH - Solid Phase Extraction MH - Vegetables/*chemistry EDAT- 2008/03/18 09:00 MHDA- 2008/09/25 09:00 CRDT- 2008/03/18 09:00 PHST- 2008/01/24 00:00 [received] PHST- 2008/02/24 00:00 [revised] PHST- 2008/02/26 00:00 [accepted] PHST- 2008/03/18 09:00 [pubmed] PHST- 2008/09/25 09:00 [medline] PHST- 2008/03/18 09:00 [entrez] AID - S0021-9673(08)00405-6 [pii] AID - 10.1016/j.chroma.2008.02.087 [doi] PST - ppublish SO - J Chromatogr A. 2008 Jul 4;1196-1197:100-9. doi: 10.1016/j.chroma.2008.02.087. Epub 2008 Mar 2.