A method for extraction and determination of trace amounts of Carbaryl, Baygon, Methiocarb, and Methiocarb sulfoxide in lettuce and apple samples is described. The arrangement liquid chromatography-particle beam-mass spectrometry offers the possibility of confirmation and determination of these carbamates at concentrations lower than those admitted by the European Union. Recoveries of carbamates at the 0.16–4.9 mg/kg level were between 53 and 76% with standard deviation between 6 and 12% (n = 5). Detection limits for analytes single ion monitoring mode were 5, 30, 10, and 20 ng for Methiocarb sulfoxide, Baygon, Carbaryl, and Methiocarb, respectively.