Abstract: A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed for the determination of anesthetic residues in fishery products. Solid-phase extraction (SPE) was used to purify and concentrate the target analytes which were separated by a HP-5MS UI column and detected in multiple-reaction monitoring (MRM) mode via positive electrospray ionization (ESI+). The results showed that the calibration curves of anesthetic residues were of good linearity in the range of 0-100 μg/L, with detection limit of 2.0 μg/kg and the quantification limit of 5.0 μg/kg in this method. The recovery was found to be 73.93%-119.97% at three spiked levels for anesthetic residues and the relative standard deviation (RSD) to be able to meet requirement of GB/T 27404-2008. The developed method is characterized by the excellent purification effect, sensitivity and accuracy, and can be used for the determination of anesthetic residues in fishery products.