A novel method was developed for the determination of methylene bisthiocyanate (MBT) in aquatic products by gas chromatography with pulsed-flame photometric detector (GC-PFPD). The samples were extracted by dichloromethane-n-hexane (1:1, v/v), concentrated and cleaned up by neutral-alumina SPE cartridges. The extracts were eluted with 8 mL dichloromethane, and blown to dryness by nitrogen at 35℃. The final extracts were redissolved with a mixture of dichloromethane-n-hexane (1:1, v/v), separated by an HP-5MS quartz capillary column (30 m×0.32 mm×0.25 μ m) and detected by PFPD with external standard method. Under the optimum experimental conditions, the standard curve was linear in the range of 1.0-20.0 mg/L with correlation coefficient of 0.9971. The limit of detection was 0.1 mg/kg. Recoveries ranged from 65.6% to 97.6% with RSDs of 6.32%-12.8% (n=7). The method has good innovative, advanced and practical values.