加速溶剂萃取-气相色谱质谱法测定海洋沉积物中多氯联苯残留

样品采用加速溶剂萃取,萃取液依次经复合硅胶和石墨化炭黑柱净化后,采用GC-MS法测定样品中的多氯联苯残留。结果表明,方法检出限为(0.005～0.038)×10-9(湿重),样品加标回收率为68.5%～108.4%,RSD为2.1%～11.8%。本方法具有提取效率高,净化效果好,回收率高,准确灵敏等优点,可应用于海洋沉积物中多氯联苯等持久性有机污染物残留的监测。

Determination of polychlorinated biphenyls residues in marine sediments using accelerated solvent extraction with gas chromatog raphy-mass spectrometry

A rapid and accurate method was developed for the determination of polychlorinated biphenyls(PCBs) residues in marine sediments by accelerated solvent extraction(ASE) and gas chromatography-mass spectrometry(GC-MS).The target analytes were extracted with hexane/acetone(1:1,v/v) by ASE and cleaned up by composite silica gel column and graphitization carbon column.The results demonstrated that the method detection limits was(0.005～0.038)×10-9 for PCBs(wet weight).The recovery percentages and RSD of two-level spiked samples were 68.5%～108.4%and 2.1%～11.8% for PCBs,respectively.The method was precise,sensitive,and highly efficient in extraction,and has been applied in the actual POPs monitoring in sediments of marine environment.