A method was developed for the determination of benzene series (BTEX) in marine sediment by headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). The conditions for extraction and gas chromatography, such as the amount of salt added, equilibrium time, extraction temperature, extraction time, desorption time and injection temperature, were optimized. The analytes were quantitatively analyzed by the internal standard method. The results showed that the linear correlation coefficients of BTEX compounds were from 0.995 to 0.999 in the range of 0.500-20.0 ng/g. The detection limits of this method were from 0.081 8 to 0. 175 ng/g, with the RSDs of inter- and intra-day of 1.2%-3.6% (n = 5) and 0.4%-6.3% (n = 3). The average recoveries under two different spiked concentrations (2.0 and 15.0 ng) were 61.7%-79.5% and 77.1%-85.6% with RSDs of 5.4%-9.6% and 3.9%-7.6% (n = 5), respectively. This method is quick, sensitive, simple, accurate and reproducible. It can be used to analyze the marine sediment samples with trace BTEX.