Abstract: The volatile compounds in hairtail were extracted by solid phase microextraction ( SPME) and analyzed by gas chromatography-mass spectrometry ( GC-MS) .In order to increase the efficiency of SPME-GC-MS, the key influencing factors of extraction efficiency were optimized with reference to the main eight volatile compounds.The results showed that the optimum extraction conditions were: 2g fish meat were homogenized with 6mL NaCl solutions ( 0.36 g /mL) in a 20 mL vial, then extracted for 50 min by 50 /30μm DVB /CAR/PDMS fiber under 50℃.Under the optimum extraction condition, a total of 40 main volatile compounds were identified in hairtail. Aldehydes, alcohols, aromatics and alkenes were the main volatile compounds, which accounted for 45.11%, 17.47%, 14.49%and 13.99%, respectively.