A method was established to determine three pesticides residues，aldicard and its metabolites aldicarb-sulfone and aldicarb-sulfoxide, in peanut oil by graphene oxide dispersive solid phase extraction (DSPE) combined with liquid chromatography-tandem mass spectrum (LC-MS/MS). The sample was extracted by acetonitrile and purified by graphene oxide with DSPE and then separated by LC with Poroshell 120 EC-C18，3.0×100mm，2.7μm column. The analysis was carried out in the multi-reaction monitoring mode and external standard method was used for quantification. The results showed that the calibration curve of the three pesticides showed a good linear relationship in the range of 5～150μg/L with the correlation coefficient r=0.991～0.999, the detection limit of the method was 0.6～1.8μg/kg, and the average recovery was 62%～103% at different level. The method is simple, fast, cheap, can meet the requirements of the determination of aldicard and its metabolites residues in peanut oil.