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液相色谱-串联质谱法同时测定尿液中 5 种拟除虫菊酯代谢物:在 39 名无已知拟除虫菊酯暴露人群中的应用。

Simultaneous determination of five synthetic pyrethroid metabolites in urine by liquid chromatography-tandem mass spectrometry: application to 39 persons without known exposure to pyrethroids.

机构信息

Department of Pharmacology and Toxicology, University Hospital, 2 Avenue Martin Luther King, 87042 Limoges, France.

出版信息

Toxicol Lett. 2012 Apr 25;210(2):248-53. doi: 10.1016/j.toxlet.2011.08.016. Epub 2011 Aug 30.

Abstract

A sensitive and reliable method was developed and validated for the determination of five synthetic pyrethroid metabolites namely cis-Cl(2)CA, trans-Cl(2)CA, Br(2)CA, 3-PBA and 4-FPBA in human urine by liquid chromatography-tandem mass spectrometry. (2)D(6)-labelled trans-Cl(2)CA and (13)C(6)-labelled 3-PBA were used as internal standards. This method was based on a liquid-liquid extraction procedure in acidic conditions using hexane solvent with a basic purification, a chromatographic separation using a specific C18 column and mass spectrometric detection in the negative polarity. Suitable limits of detection (0.015μg/L for the five compounds) and quantification (from 0.020 to 0.030μg/L) were obtained for rendering the method usable for the biomonitoring of pyrethroids in the general population. The efficiency of the method was tested in 39 urine samples from French people without any known exposure to pyrethroids. At least three of the five metabolites were detected in each sample. The results of this study were compared to those obtained in previous ones and discussed.

摘要

建立并验证了一种灵敏、可靠的方法,用于通过液相色谱-串联质谱法测定人尿液中 5 种合成拟除虫菊酯代谢物,即顺式-Cl(2)CA、反式-Cl(2)CA、溴(2)CA、3-PBA 和 4-FPBA。(2)D(6)标记的反式-Cl(2)CA 和(13)C(6)标记的 3-PBA 被用作内标。该方法基于在酸性条件下使用正己烷溶剂进行液-液萃取,碱性净化,使用特定的 C18 柱进行色谱分离,以及在负极性下进行质谱检测。该方法的检测限(5 种化合物的检测限为 0.015μg/L)和定量限(0.020-0.030μg/L)都适合,可用于监测普通人群中拟除虫菊酯的生物监测。该方法的效率在 39 份来自法国、无已知拟除虫菊酯暴露的人的尿液样本中进行了测试。在每个样本中至少检测到 5 种代谢物中的 3 种。本研究的结果与之前的研究结果进行了比较和讨论。

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