A new GC-QqQ–MS/MS method was developed to determine the polycyclic aromatic hydrocarbons (PAHs) in fish. In this method, the samples were pretreated by ultrasonic extraction with hexane/dichloromethane and purified with hexane/acetone on florisil column, and then analyzed on a TR-5MS column. PAHs can be detected in the modes of electron impact ionization and selective reaction monitoring. The calibration curves had good linearity within 0.4~50 μg/kg for each pesticide (0.9999＞R＞0.9865). The limits of the detection ranged from 0.024 μg/kg to 0.06 μg/kg and the limits of quantitation ranged from 0.08 μg/kg to 0.2 μg/kg. The recoveries of PAHs varied from 68.5% to 106.3% with the relative standard deviations of 0.3~17.8% at the spiked levels 5, 10 and 50 μg/kg. It was satisfied with successfully determination of fish samples by this analytical approach.