A dispersive solid phase extraction coupled with gas chromatography-mass spectrometry (GC-MS) method was established for the determination of trace amounts of musk ketone in aquatic products. The target analyte in the samples was extracted with acetonitrile containing 1% acetic acid, cleaned-up with the mixture of N-propyl-ethylenediamine (PSA), C18 and graphitized carbon (GCB), and analyzed by GC-MS under selected ion monitoring (SIM) mode and quantified by the external standard method. The orthogonal experiment was carried out to optimize the pre-treatment conditions. Under the optimal conditions, good linear relationship was obtained in the range of 1 - 50 microg/L for musk ketone with correlation coefficient not less than 0.999, and the limits of detection (S/N = 3) was 0.30 microg/kg. The recoveries of musk ketone in the prawn and tilapia blank samples at three spiked levels of 1.0, 2.0 and 10.0 microg/kg ranged from 91.8% to 110.6% with RSDs in the range of 2.6% - 8.4%. The method is simple, rapid and accurate, and can be used for the routine analysis of musk ketone in aquatic products.