PMID- 16372385 OWN - NLM STAT- MEDLINE DCOM- 20060323 LR - 20061115 IS - 0951-4198 (Print) IS - 0951-4198 (Linking) VI - 20 IP - 3 DP - 2006 TI - Validation of a gas chromatography/triple quadrupole mass spectrometry based method for the quantification of pesticides in food commodities. PG - 365-75 AB - A new multiresidue method has been validated in cucumber matrix for the routine analysis of 130 multiclass pesticide residues by gas chromatography/triple quadrupole mass spectrometry. The pesticides were extracted with ethyl acetate. A first identification of the pesticides was based on a tandem mass spectrometric (MS/MS) screening method, which monitors a single transition for each target compound, in less than 12 min. After that, potentially non-negative samples were analyzed again by the MS/MS confirmation/quantification method, which monitors two or three MS/MS transitions for each compound, also in less than 12 min. Performance characteristics, such as trueness, precision, linear range, detection limit (LOD) and quantification limit (LOQ), for each pesticide were calculated. The average recoveries obtained ranged between 70 and 120% at three different fortification levels (25, 200 and 500 microg/kg) with precision, expressed as relative standard deviation (RSD), values lower than 15%. The calculated LOD and LOQ were typically <3.2 and 9.6 microg/kg, respectively. Such limits were much lower than the maximum residue levels (MRLs) established by European legislation. The proposed methodology was applied to the determination of pesticides in real vegetable samples from Almeria (Spain). CI - Copyright (c) 2005 John Wiley & Sons, Ltd FAU - Martinez Vidal, J L AU - Martinez Vidal JL AD - Department of Analytical Chemistry, University of Almeria, 04071 Almeria, Spain. FAU - Arrebola Liebanas, F J AU - Arrebola Liebanas FJ FAU - Gonzalez Rodriguez, M J AU - Gonzalez Rodriguez MJ FAU - Garrido Frenich, A AU - Garrido Frenich A FAU - Fernandez Moreno, J L AU - Fernandez Moreno JL LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - England TA - Rapid Commun Mass Spectrom JT - Rapid communications in mass spectrometry : RCM JID - 8802365 RN - 0 (Pesticides) SB - IM MH - Calibration MH - Food Contamination/*analysis MH - Gas Chromatography-Mass Spectrometry MH - Molecular Structure MH - Pesticides/*analysis/isolation & purification MH - Reference Standards MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Vegetables/chemistry EDAT- 2005/12/24 09:00 MHDA- 2006/03/24 09:00 CRDT- 2005/12/24 09:00 PHST- 2005/12/24 09:00 [pubmed] PHST- 2006/03/24 09:00 [medline] PHST- 2005/12/24 09:00 [entrez] AID - 10.1002/rcm.2315 [doi] PST - ppublish SO - Rapid Commun Mass Spectrom. 2006;20(3):365-75. doi: 10.1002/rcm.2315.