Abstract: A method for the determination of organophosphorous pesticide residues in a supporting solution of 0.40 mol/L sodium hydroxide by single sweep polarography has been established. The Peak potentail is -0.53 V(vs.SCE). The peak height is linearily proportional to the concentration of phoxim over the range of 0.12～160 μg/mL, 0.15～200 μg/mL methyl parathium,0.20～160 μg/mL isocarbophos, 0.10～1.0 mg/mL methamidophos, 0.09～160 μg/mL flolimat. This proposed method is simple, sensitive and has good selectivity. The results are satisfactory when it is used to analyse vegetablefruit.