Abstract: A method of gas chromatography coupled with triple quadrupole mass spectrometry (GC-MS/MS) was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in marine sediments, and isotope dilution was introduced to quantification of PAHs. The results were compared with those obtained by gas chromatography coupled to mass spectrometry (GC-MS). The more accurate quantification results, and better selectivity and sensitivity of PAHs were obtained with GC-MS/MS than GC-MS. The recoveries of spiked samples ranged from 71% to 105%, the recoveries of 16 deuterated-PAHs ranged from 55% to 101%. The GC-MS/MS method was applied to analyzing the real marine sediment of Liaodong bay, and the results showed that the relative standard deviation of parallel samples ranged from 2.2% to 4.9%, and the concentration of individual PAHs in sediment samples ranged from 0.25×10^-9 (dry weight) to 30.1×10^-9 (dry weight).