A gas chromatography－triple quadrupole mass spectrometry was developed for the rapid determination of pyroxasulfone residues in animal-derived foods．Pyroxasulfone residues in pork，pig liver，chicken，chicken liver，milk and eggs were extracted with acetonitrile，and cleaned up with primary-secondary amine，stearyl bonded silica gel and anhydrous magnesium sulfate as dispersive solid-phase extraction sorbent．After centrifugation，the supernatant liquid was nitrogen-blowed to dryness．After redissolved with acetone and filtered，the analyte was detected by gas chromatography－triple quadrupole mass spectrometry，and quantified by external standard method．The instrument conditions，extraction solvents and purification method were optimized in the experiment，and the optimal pretreatment method and instrument conditions were obtained．The detection effects of pyroxasulfone by triple quadrupole liquid chromatography－mass spectrometry and triple quadrupole gas chromatography－mass spectrometry were compared．The results showed that the response of pyroxasulfone on triple quadrupole liquid chromatography－mass spectrometry was poor，and the detection sensitivity could not meet the requirements of relevant regulations，while the detection effect of pyroxasulfone by triple quadrupole gas chromatography－mass spectrometry was excellent，which could meet the detection requirements．In addition，the extraction effects of hexane，acetone，ethyl acetate，acetonitrile and acidic acetonitrile as extraction solvents were compared，and the results showed that acetonitrile was the most suitable extraction solvent．The matrix effect of the sample was investigated，and it was found that the matrix effects of pyroxasulfone in the six matrices were less than 20%，which were a weak matrix effect without compensation. Under the optimal conditions，the calibration curve was linear in the range of 0.5－100 µg/L with correlation coefficients of 0.999 5． The limit of quantitation was 0.001 mg/kg. The average recoveries for blank samples at low，medium and high spiked levels ranged from 85.8% to 106%，with relative standard deviations（,n ,= 6） of 3.1%－6.8%．This method was used to determine 50 animal-derived foods，in which pyroxasulfone residues were detected in one beef sample and one mutton sample．The method is simple，rapid and sensitive，and it could meet the requirements for detection of pyroxasulfone residue in animal-derived foods.