Abstract: A rapid method for determination of nereistoxin pesticides in animal tissues by GC-MS/MS with accelerated solvent extracted was proposed.The animal tissue sample (e.g.blood,liver and etc.) was extracted with a mixture of cyclohexane,acetone and dichloromethan (mixed in the ratio of 1 to 1 to 1 by vol.) to transfer the pesticides into the organic phase.On-line purification with aluminum oxide was used to remove impurities from the extract.The extract was evaporated to dryness in a water bath at 40 ℃,and the residue was taken up with 2.0 mL of methanol,which was used for GC-MS/MS determination.Two pesticides,i.e.,bisultap and chlordimeform,were determined by the proposed method,giving linearity ranges between 2.4-7.2 mg·L-1 and 1.2-7.2 mg·L-1 respectively.Detection limits (3S/N) of 48 μg·L-1 (for bisultap) and 8 μg·L-1 (for chlordimeform) were obtained.Recovery and precision were tested by the standrad addition method and the results obtained were as follows:values of average recovery:92.0% and 90.0% for bisultap in blood and liver samples,93.0% and 92.7% for chlordimeform in blood and liver samples respectively;values of RSD′s (n=6):2.1% and 4.5% in the former case;3.5% and 6.9% in the latter case.