Multiresidue determination of pesticides in agricultural products by gas chromatography/mass spectrometry with large volume injection

Abstract

A method is described for the rapid determination of pesticide residues in agricultural products. Pesticides were extracted from samples with acetonitrile. To remove pigments and fatty acids, an aliquot of the extract was cleaned up by a minicolumn that was packed both with graphitized carbon black and primary secondary amine. Analysis was performed by gas chromatography/ mass spectrometry with programmable temperature vaporizer-based large volume injection using a liner packed with phenylmethylsilicone chemically bonded silica. The method was evaluated for 114 pesticides by spiking into tomato, spinach, Japanese pear, grape, and brown rice at various concentrations of each pesticide (0.02-0.4 μg/g). The method, which gave good recovery (>60%) for 108 pesticides, is characterized by high cleanup efficiency and short cleanup time, and is useful as a rapid screening analysis.