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研究了加速溶剂萃取底泥中多氯联苯残留的最佳条件和净化方法。研究表明,采用正己烷—丙酮混合溶剂(体积比1∶1)为提取剂,萃取温度100℃,压力为10.3 Mpa,分别采用浓硫酸法和弗罗里硅土固相萃取柱对样品净化,毛细管柱分离,配有电子捕获检测器的气相色谱(GC-ECD)进行检测,平均加标回收率为92.4%~102%,相对标准偏差(RSD,n=11)为0.98%~4.30%,检出限为0.77~1.72 ng/g,方法简单、快捷、经济,适应于底泥中多氯联苯的测定。
The optimum conditions and purification methods for accelerating PCB residues in solvent-extracted sediment were studied. The results showed that the extraction temperature was 100 ℃ and the pressure was 10.3 Mpa by using n-hexane-acetone mixed solvent (volume ratio 1: 1) as extractant. The samples were purified by concentrated sulfuric acid method and Florisil solid-phase extraction (SPE) The average recoveries were 92.4% -102% and the relative standard deviations (RSDs, n = 11) were 0.98% -4.30% by GC-ECD with capillary column separation and gas chromatography with electron capture detector (GC- The detection limit was 0.77 ~ 1.72 ng / g. The method was simple, rapid and economical, and suitable for the determination of polychlorinated biphenyls in sediment.