气相色谱-质谱法检测人血清样品中新型含氯阻燃剂德克隆

Quantification of Dechlorane Plus in Human Serum by Gas Chromatography Coupled with Negative Chemical Ionization Mass Spectrometry

采用液液萃取,气相色谱-负离子化学电离质谱技术,建立了人体血清样品中新型含氯阻燃剂德克隆(DP)的分离分析方法。血清样品蛋白质变性后,采用液液萃取法提取脂肪,再采用浓H2SO4破坏法去除大部分脂肪,最后采用酸性硅胶柱进一步净化。净化后的样品经浓缩富集,采用气相色谱-负离子化学电离质谱仪测定样品中DP两种同分异构体的含量。结果表明:本方法的加标回收率为70.2%～85.7%;仪器检出限为0.5～0.7 pg;方法检出限为15～20 pg,适合实际样品中该类污染物的分离分析。采用本方法测定了某电子垃圾拆解工人和对照区居民血清中的DP浓度水平,分别为7.8～465 ng/g脂肪和0.93～50.5 ng/g脂肪。

A gas chromatography coupled with negative chemical ionization mass spectrometric（GC-NCI-MS） method was developed for the determination of two dechlorane plus（DP） isomers in human serum sample.Target compound and serum lipid were extracted by lipid-lipid extraction.After the sulfuric acid treatment to remove extracted lipids from the samples,samples were further cleaned up with a silica/sulfuric acid column.Identification and quantification of DP were carried out by MS.The detection limit of instrument was 0.5-0.7 pg.The detection limit of the method was 15-20 pg per sample.Spiked recoveries of DP in human serum samples were in the range of 70.2%-85.7%.The developed method was further validated in human serum.DP concentrations were analyzed in 20 electronics dismantling workers and 20 reference humans,total DP concentration was 7.8-465 ng/g lipid and 0.93-50.5 ng/g lipid,respectively.