高通量固相萃取-GC/MS法测定水源水中多氯联苯

High-throughput solid phase extraction coupled GCMS method for determination of Polychlorinated biphenyls(PCBs)in source water

建立了高通量全自动固相萃取-气相色谱质谱法同时测定水中9种多氯联苯(Polychlorinated biphenyls,PCBs)的分析方法。水样经高通量全自动固相萃取仪进行富集,优化上样流速,洗脱溶剂类型以及洗脱溶剂体积,确定最优的全自动固相萃取条件。结果表明:在10-200μg/L范围内,线性关系良好,9种多氯联苯相关系数为0.9990-09996,方法检出限为0.0289-0.2691μg/L。空白样品加标浓度为0.1μg/L时,平均加标回收率为85.4%-90.6%,相对标准偏差(n=6)为0.67%-5.21%。将该方法用于惠州市虾村水源水,菱湖以及鳄湖的实际水样测定,结果9种多氯联苯均未检出,说明以上三个引用水源水没有受到PCBs的污染。

Here an analytical method which utilized high-throughput automated solid phase extraction coupled GCMS was established for simultaneous determination of 9 Polychlorinated biphenyls(PCBs).The mentioned water sample was enriched by automated solid phase extraction system with the optimized the experimental parameter as loading flow rate,elution solvent,and elution solvent volume.After the optimization,the determination result showed that the method present good linear correlation for 9 PCBs in the linear range of 10-200μg/L.The coefficient of 9 PCBs were 0.9990~09996,the detection limits were 0.0289~0.2691μg/L.For method validation,spiked blank samples(0.1μg/L)and actual source water sample were determined respectively.The average recovery of spiked 9 PCBs samples ranged 85.4%~90.6%with RSD(n=6)0.67%~5.21%.The result for actual source water sampled from Xia Village,Linghu Lake and Crocodile Lake in Huizhou City were all not detected of 9 PCBs,indicating the source water in above mentioned sites were not affected by PCBs pollutant.