Abstract: In this experiment, an analytical method for the determination of 16 PAHs in fried squid by ultrasonic extraction-gas chromatography-mass spectrometry (PAHs) was established. The effects of extraction reagent ratio, extraction reagent dosage and extraction temperature on the recovery rate were investigated. The best extraction and detection method was determined as follows: after freeze-drying, 5.00 g sample was extracted by 25 mL n-hexane at 30 ℃ for 20 min, and then reextracted once. After purification by alkaline alumina neutral silica gel composite solid phase extraction column, compounds was determined by gas chromatography tandem mass spectrometry and quantified by deuterium internal standard method. Under these experimental conditions, 16 target compounds showed good linear relationship in the range of 1~100 ng/mL, the linear correlation coefficient (r) was not less than 0.9994, the detection limit was 0.09~0.52 μg/kg, and the quantitation limit was 0.21~1.21 μg/kg. The recoveries were 73.98%~128.17%, 73.21%~133.24% and 76.35%~133.68% at the spiked levels of 1, 2 and 20 μg/kg, respectively. The relative standard deviations (RSD, n=6) were 1.32%~2.98%, 0.93%~2.47% and 1.08%~2.87%, respectively. In the actual sample detection application, PAHs were detected in all the six samples. The detection range of single component ranged from 0 to 48.65 μg/kg. The results showed that the method had good selectivity. It could be used for the detection of polycyclic aromatic hydrocarbons in fried squid and other similar processed aquatic products.