The mesylate derivatives of the carbamate pesticides propoxur, thien-4-yl methylcarbamate), Landrin, Carbaryl, carbofuran, 3-hydroxycarbofuran, 3-oxocarbofuran, methiocarb, methiocarb sulfoxide, and methiocarb sulfone were prepared and found to be suitable for the gas chromatographic detection of these pesticides. The carbamate pesticide is hydrolyzed with methanolic KOH, and the resultant phenol reacted with methanesulfonyl chloride and pyridine to form the mesylate derivative, which is determined by a gas chromatograph equipped with a flame photometric detector in the sulfur mode. This method is highly specific and free from interference of extracted crop materials. This procedure was applied to the determination of carbaryl residues in lentil straw. Recoveries of carbaryl from lentil straw samples fortified with the pure pesticide at the rate of 0.1 ppm averaged 103.0% (range 91.0-118.0%).