Splitless large-volume GC-MS injection for the analysis of organophosphorus and organochlorine pesticides in vegetables using a miniaturised ethyl acetate extraction

A simple, rapid and sensitive multiresidue method has been developed for the determination of ten organophosphorus and organochlorine pesticides, commonly used in crop protection. The analysis uses a miniaturised extraction with ethyl acetate followed by large volume injection (10 mu L) GC-EI-MS analysis in SIM (selective ion monitoring) mode. Sensitivity and selectivity of the method were acceptable with limits of detection (LODs) lower than 0.01 mg kg(-1), except for endosulfan alpha and beta (0.05 mg kg(-1)). Average recoveries of between 63-99% were obtained and good linearity was observed in the range from 0.01 to 1.00 mg kg(-1). Repeatability and reproducibility studies yielded relative standard deviations lower than 20% in all the cases. The method was applied to the analysis of 110 tomato, pepper and cucumber samples, as part of the monitoring programme of the Association of Producers and Exporters of Fruits and Vegetables of Almeria.