Abstract: Objective To establish a rapid qualitative method for determination of acetamiprid in blood and gastric juice. Methods Acetamiprid in the samples were extracted by dichloromethane, then the organic phase was evaporated by nitrogen stream; the remains were dissolved with dichloromethane to constant volume and detected by GC-MS. Results The detection of acetamiprid in blood and gastric juice can be completed in 90 min. The qualitative analysis can be done by the comparison of total ion chromatograms and mass spectrums of the samples with the standard mass spectra. Conclusion The method can identify acetamiprid ingredients in the blood and gastric juice rapidly and accurately.