海洋沉积物中多氯联苯、多环芳烃和有机氯农药的同时净化与分离

Simultaneous Purification and Separation of Polychlorinated Biphenyls,Polycyclic Aromatic Hydrocarbons and Organochlorine Pesticides in Marine Sediments

研究了海洋沉积物提取液中28种多氯联苯（PCBs）、16种多环芳烃（PAHs）和21种有机氯农药（OCPs）在硅胶-氧化铝复合净化柱上的同时净化与分离效果,结果表明：在充填4 cm3%去活化氧化铝-6 cm 3%去活化硅胶的8 mm i.d×15 cm固相萃取净化柱上,使用10 mL正己烷作为淋洗PCBs的分割点,可实现PCBs、PAHs和OCPs的满意分离,更有利于PCBs与高环数PAHs、极性较强OCPs的分离。继续用20 mL正己烷-二氯甲烷混合液（体积比1∶1）洗脱,28 PCBs、16种PAHs和21种OCPs均可获得有效回收,回收率分别为75%-110%、76%-115%、75%-130%。经海洋沉积物标准参考物质验证,该方法实用、可靠,流程简单,试剂消耗少,成本低,适用于海洋环境地质调查中基质复杂沉积物样品的定量分析。

Simultaneous purification and separation of 28 polychlorinated biphenyls（PCBs）,16 polycyclic aromatic hydrocarbons（PAHs） and 21 organochlorine pesticides（OCPs） in marine sediment extracts by using solid-phase extraction（SPE） column of alumina-silica gel is presented in this paper.The results indicate that using 4 cm 3% deactivated alumina and 6 cm 3% deactivated silica gel and cutting off PCBs collection after loading 10 mL C6H14 eluting solvent through the 8 mm i.d.×15 cm column can yield satisfactory separation of PCBs,PAHs and OCPs,especially between PCBs and higher cyclic PAHs and higher polarity OCPs.All 65 kinds of PCBs,PAHs and OCPs can be completely recovered with being continuously eluted by 20 mL C6H14/CH2Cl2（V/V,1∶1）.All of 65 kinds of PCBs,PAHs and OCPs can be effectively recoveried,and the recoveries are ranged from 75% to 110%,76% to 115% and 75% to 130%,respectively.Using marine sediment standard reference materials,the method provides the advantages of being practical,reliable,easy to operate,having low reagent consumption,low cost,etc.,and is very suitable for the quantification of marine sediment samples with complicated matrices during marine environmental geology surveys.