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

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

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。

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 PC Bs （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.