In this work, some carbamate pesticides were extracted from aqueous sample using single drop microextraction. Extraction was performed using a 3.5 ?L benzonitrile droplet hanging from needle tip of a 10 ?L GC syringe from 5 ml sample solution. Propoxure, pirimicarb, carbaryl, carbofuran, desmsdipham, phenmedipham, methiocarb and thiofanox were studied carbamates. Two different procedures were used to inject extracted carbamates in to GC-MS. First, extracted sample was injected using cold on-column into the GC-MS. In the second method, carbamates in sample were derivatized using acetic anhydride as derivatization agent in a capillary tube. Then derivatized sample injected in to the GC-MS using splitless injection port. Derivatization reaction conditions were studied and optimized. Derivatization reaction was performed using 0.7 ?L volume of acetic anhydride at 150°C during 120 min. Experimental parameter such as solvent type, extraction time, extraction temperature, solution pH were studied. The best extraction efficiency was obtained using benzonitrile as extraction solvent, 3.5 ?l volume of organic solvent, stirring rate of 250 rpm, 15 min extraction time, whitout adding of NaCl in neutral sample pH at room temperature. For cold on-column reproducibility ranging from 4.7 to 8.3% and the limits of detection (LODs) ranged between 0.03 and 0.08 ?g L -1 using GC–MS with selective ion monitoring. For splitless condition reproducibility ranging from 3.2 to 8.3% and the limits of detection (LODs) ranged between 0.003 and 0.035 ?g L -1 using GC–MS with selective ion monitoring.
