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

发布时间：2018-07-06 08:41

本文选题：内分泌干扰物 + 超高效液相色谱-串联质谱　；参考：《分析化学》2017年03期

【摘要】：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 m L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,除均二苯脲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。
[Abstract]:A multi-objective analysis method for 9 trace endocrine disruptors (EDCs) in biological samples was established. Vortex oscillation-ultrasonic assisted extraction, combined with gel permeation chromatography (GPC), was used to remove the interference of macromolecular organic matter, and then purified by silica gel column chromatography. Finally, the mobile phase of the mixture of ethyl acetate and cyclohexane (1: 1 V / V) was determined by UHPLC-MS / MS, and 1228 mL was selected as the collection section of the target compound fraction. The electrospray ion source positive ion mode and atmospheric pressure chemical ionization source negative ion mode are used in the mass spectrometry, and the data acquisition is a multiple reaction monitoring mode. The recoveries of the method were 65.2 and 118.0, and the quantitative limit was 0.1 ~ 9.7 ng/g 路dw (dry weight). This method was used to analyze the endocrine disrupting pollutants in carp ridge meat of Pearl River water system. The results showed that the contents of other endocrine disrupting pollutants were 0.1 ~ 22.6 ng/g / dw except for diphenylurea and trichlorocarban.
【作者单位】：中国科学院广州地球化学研究所有机地球化学国家重点实验室;中国科学院大学;
【基金】：国家自然科学基金资助项目(Nos.41372358,41572330)~~
【分类号】：X835;O657.63

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