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Validation of a multiclass multiresidue method and monitoring results for 210 pesticides in fruits and vegetables by gas chromatography-triple quadrupole mass spectrometry
Authors:Samanta Uclés  Noelia Belmonte  Ana B Martínez  M Jesus Martinez-Bueno  Miguel Gamón
Institution:1. Agrifood Campus of International Excellence (ceiA3), European Union Reference Laboratory for Pesticide Residues in Fruit &2. Vegetables, University of Almeria, Almería, Spain;3. Hydrosciences Montpellier UMR 5569, Department of Environmental Sciences and Public Health, University of Montpellier I, Montpellier, France;4. Pesticide Residue Laboratory (Agro-Food Analysis Service) of the Generalitat Valenciana, Burjassot, Valencia, Spain
Abstract:A rapid, sensitive, accurate and reliable multiresidue method for the identification and quantification of 210 relevant pesticides in four representative fruit and vegetable commodities (tomato, potato, spring onion and orange) has been developed and validated by gas chromatography in tandem with triple quadrupole mass spectrometry. The method has been fully validated and applied to 292 samples from different countries. Prior to instrumental analysis, an extraction procedure based on a sample extraction of multiclass analytes, using the ethyl acetate method was employed. Mass spectrometric conditions were individually optimized for each compound in the selected reaction monitoring (SRM) mode to achieve maximum sensitivity. The pesticides were separated in less than 25 min. This was followed by an exhaustive control of the retention times. The Retention Time Locking Method was applied, working at a constant pressure throughout the analysis. System maintenance was reduced by using a purged capillary flow device that provided backflush capabilities by reversing column flow immediately after elution of the last compound of interest. Istotopically labelled internal standards were employed to improve the quality of the analytical results.
Keywords:Multiresidue methods  GC-QQQ-MS  fruits and vegetables  pesticides  monitoring
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