建立了加速溶剂萃取/气相色谱-质谱法(ASE/GC-MS)同时测定海洋沉积物中28种多氯联苯(PCBs)、16种多环芳烃(PAHs)和21种有机氯农药(OCPs)的分析方法.结果表明,ASE的最佳萃取温度为100 ℃,最佳静态时间为5 min.GC-MS同时分析65种化合物时,PAHs的线性范围为0.05 ～5.00 mg/L,线性系数(r2)为0.991 ～0.999;PCBs和OCPs的线性范围为5.0 ～500.0 μg/L,r2不低于0.996.PCBs、PAHs和OCPs的检出限分别为0.03 ～0.11、0.04 ～0.73、0.06 ～0.48 μg/kg,定量下限分别为0.11 ～0.35、0.12 ～2.42、0.18 ～1.61 μg/kg,平均加标回收率为70% ～146%,方法的相对标准偏差(n=6)为1.2% ～17.3%.经海洋沉积物标准参考物质验证,该方法高效、准确,适合海洋沉积物中65种化合物的同时定量分析.%A gas chromatography - mass spectrometry ( GC - MS) coupled with accelerated solvent extraction(ASE) method was developed for the simultaneous determination of 28 polychlorinated biphenyls, 16 polycyclic aromatic hydrocarbons and 21 organochlorine pesticides in marine sediments. The results indicated that the best simultaneous extraction temperature and time were 100 ℃ and 5 rain, respectively. Under the optimal conditions, the analysis of 65 compounds were carried out with GC - MS. The calibration curves were linear in the range of 0. 05 - 5.00 mg/L for PAHs with correlation coefficients( r2 ) of 0. 991 - 0. 999 and 5.0 - 500. 0 μg/L for PCBs and OCPs with r2 no less than 0. 996. The limits of detection of PCBs, PAHs and OCPs were in the range of 0. 03 - O. 11, 0.04 -0. 73, 0.06 -0.48 1μg/kg, and the limits of quantitation were in the range of O. 11 - 0.35, O. 12-2.42, O. 18 -1.61 1μg/kg, respectively. The spiked recoveries ranged from 70％ to 146％ with RSDs(n =6) of 1.2％ - 17.3％ for all the compounds. Through marine sediments standard reference materials, the method was proved to be effective and accurate, and could be applied in the simultaneous determination of 65 compounds in marine sediments.
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