| A GC-MS method was developed and validated for the determination of sixteen polycyclic aromatic hydrocarbons(PAHs) listed by the US Environmental Protection Agency as priority pollutants in marine organisms such as fish,shrimp,mussel,crab and the others.The procedures of extraction and purification,as well as chromatographic and mass spectrometric parameters,were optimized.The biological samples were extracted ultrasonically with hexane-dichloromethane(2∶1) mixture,and treated with 60% sulfuric acid,followed by clean-up with a glass column containing Florisil and neutral alumina.The analysis of target compounds was performed by gas chromatography-mass spectrometry(GC-MS).Under the optimized conditions,the calibration curves of 16 PAHs were linear in the range of 0.005-0.500 mg/L with correlation coefficients(r) not less than 0.998 4 and limits of detection of 0.03-0.28 μg/kg.The average spiked recoveries for the fishery products at the spiked levels of 2,20 and 100 μg/kg were in the range of 55%-118%,80%-114% and 79%-113%,respectively,with relative standard deviations(RSDs,n=6) less than 10%.The results showed that the method is rapid,accurate,sensitive and reliable,and could satisfy the requirements for analysis on persistent organic pollutants(POPs) in marine organisms. |