A liquid chromatography–mass spectrometry (LC–MS) method was established for the purpose of simultaneous determination of carbamate and organophosphorus (OPPs) pesticides in fruits and vegetables. Samples were extracted with acetonitrile; and then prepared by dispersive solid-phase extraction (dispersive-SPE) with primary secondary amine (PSA) as the sorbent. Four common representative samples (tomato, apple, carrot, and cabbage) were selected from the supermarket to investigate the effect of different matrices on pesticides recoveries and assay precision after spiking
samples with 0.05 mg/kg. Matrix composition did not interfere significantly with the determination of the pesticides. The obtained recoveries were, with a few exceptions, in the range of 70–110% with RSDs less than 8%. It was applied to pesticide residue monitoring in vegetables and fruits
from local markets.