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建立了微波消解-基质固相分散萃取-高效液相色谱法测定水产品中中16种多环芳烃(PAHs)的分析新方法。优化的前处理方法为5.0 g样品加入10 m L二氯甲烷、10 m L正己烷进行微波萃取,取10 m L提取液氮吹至约近干,以乙腈定容至1.0 m L,分别加入200 mg PSA,200 mg C18,200 mg无水硫酸镁净化后进行色谱分析,方法的检出限范围为0.20~2.00μg/kg,相对标准偏差分别在4.0%~17%,相关系数区间为0.9990~0.9999;利用此方法对虾蛄和梭子蟹样品进行测定,发现不同组织间的浓度差异表达为内脏团>壳>肌肉,多环芳烃的主要组成为萘、菲和芘。
A new analytical method for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in aquatic products was established by microwave digestion-matrix solid-phase dispersion extraction-high performance liquid chromatography. The optimized pretreatment method is that 5.0 g sample is added with 10 m L dichloromethane and 10 m L n-hexane for microwave extraction. The extract is extracted with 10 m L of nitrogen to nearly dry nitrogen and fixed with acetonitrile to 1.0 mL. 200 mg PSA, 200 mg C18 and 200 mg anhydrous magnesium sulfate. The detection limits were 0.20 ~ 2.00 μg / kg with relative standard deviations (RSDs) of 4.0% ~ 17% and correlation coefficients of 0.9990 ~ 0.9999. Using this method, the samples of shrimp shrimp and shuttle crab were determined and the difference in concentration among different tissues was expressed as visceral mass> shell> muscle. The main components of PAHs were naphthalene, phenanthrene and pyrene.