A method was developed for the determination of 46 pesticides in sulfur-containing vegetables(e.g.scallion,ginger,Chinese chives and garlic) using solid-phase extraction(SPE) and gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS).The extraction solvent,solid-phase extraction column and elution solution were optimized.The pesticides were extracted with acetonitrile containing 1% acetic acid,and then cleaned up on a Carbon/NH2 SPE column.The extracts were determined by GC-MS/MS under multiple reaction monitoring(MRM) mode with the external standard method.The calibration curves of 46 pecitides were linear in the range of 0.05-1.00 mg/L with limits of detection(LOD) of 0.001-0.003 mg/kg.The recoveries of all pesticides at the spiked levels of 0.01,0.05,0.10 mg/kg in matrices were in the range of 60%-125%,with relative standard deviations(RSDs) not more than 17.3%.The method covers many kinds of pesticides(e.g.organophosphates,organochlorines and pyrethroids),with high sensitivity but low background.Therefore,it is suitable for the analysis of pesticide residues in sulfur-containing vegetables. |