超高效液相色谱-串联质谱多目标分析生物样品中的微量内分泌干扰污染物

建立了生物样品中9种微量内分泌干扰物(EDCs)的多目标分析方法.采用旋涡振荡-超声波辅助萃取,结合凝胶渗透色谱(GPC)除去大分子有机物干扰,再经硅胶柱层析进一步净化,最后应用超高效液相色谱-串联质谱(UHPLC-MS/MS)检测.GPC采用乙酸乙酯-环己烷混合溶液(1:1,V/V)为流动相,选择12~28 mL为目标化合物馏分的收集段;质谱采用电喷雾离子源正离子模式和大气压化学电离源负离子模式,数据采集为多重反应监测模式.方法回收率为65.2%~118.0%,定量限为0.1~9.7 ng/g dw(干重).采用本方法初步分析了珠江水系鲤鱼脊肉中的内分泌干扰污染物,结果表明,除均二苯腺和三氯卡班未被检出外,其它内分泌干扰污染物的含量为0.1~22.6 ng/g dw.

Multi-target Determination of Trace Endocrine Disrupting Chemicals in Biota Using Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

An ultra-high performance liquid chromatography-tandem mass spectrometry ( UHPLC-MS/MS ) method was developed and validated for the simultaneous determination of 9 kinds of trace endocrine disrupting chemicals in biological samples using ultrasonic-assisted extraction followed by purification with gel permeation chromatography ( GPC) and silica gel columns. The sample extracts were purified by Bio beads S-X3 GPC columns with cyclohexane/ethyl acetate (1:1, V/V) as mobile phase, and the target compounds were eluted in the fraction of 12-28 mL retention volume. Electrospray ionization source operated in positive mode and atmospheric pressure chemical ionization source operated in negative mode were used for mass spectrometric detection. Data acquisition was carried out in multiple reaction monitoring mode. Recoveries were predominately within 65 . 2%-118 . 0%. Method quantification limits were 0 . 1-9 . 7 ng/g dw ( dry weight ) . This method was successfully applied to the analysis of the target endocrine disrupting chemicals in carps collected from the Pearl River. with the exception of carbanilide and triclocarban, the rest analytes were detected in fish tissue samples, with the concentrations varied within the range of 0. 1-22. 6 ng/g dw.