Abstract: The residue analytical method of two organophosphorus pesticides (methamidophos and omethoate) and one carbamate pesticide (carbofuran) in cucumber and lettuce was studied. The florisil was mixed with the homogenized vegetable samples. The florisil mixture column was used in the pretreatment of the samples. The eluted solvent was concentrated and directly detected by GC NPD. This method was further used for the determination of the pesticides residue in the treated vegetables. The fortified recoveries and the detection results showed that the extraction and cleaning up procedures were good, and the method has good repeatability and sensitivity. It is a rapid and precise analytical method of those pesticides in vegetables.