A method using gas chromatography (GC) was developed to determine insecticide dialifos in agricultural products. Dialifos were extracted with acetone, the filtrate was evaporated to 50 mL and mixed with 50 mL of petroleum ether; the mixture was then extracted with dichlormathane twice. The extracts were evaporated to dry, dissolved in acetone, and then determined by gas chromatography equipped with a flame photometric detector (FPD) and a DB-1 capillary column. Recovery studies were carried out by spiking the standard dialifos at the levels of 0.05~0.15, 0.5~1.5 and 0.5~1.5 ppm to rice, citrus fruit and kiwi fruit, respectively. Average recoveries were 88.5~93.4%, 94.4~97.0% and 93.0~99.7% and the detection limits were 0.01, 0.05 and 0.05 ppm, respectively. No residue of dialifos was detected in agricultural products which were sampled from traditional markets.