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采用固相萃取和超高效液相色谱-串联质谱联用技术(UPLC-MS/MS)对有机磷酸酯阻燃剂的九种尿液代谢物进行定量测定。

Quantitative determination of nine urinary metabolites of organophosphate flame retardants using solid phase extraction and ultra performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS).

作者信息

Kosarac Ivana, Kubwabo Cariton, Foster Warren G

机构信息

Environmental and Radiation Health Sciences Directorate, Health Canada, Ottawa, ON K1A 0K9, Canada.

Environmental and Radiation Health Sciences Directorate, Health Canada, Ottawa, ON K1A 0K9, Canada.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Mar 1;1014:24-30. doi: 10.1016/j.jchromb.2016.01.035. Epub 2016 Jan 28.

Abstract

Over the last few years, the use of organophosphate flame retardants (OPFRs) has been on the rise; however, there are knowledge gaps in both the human health effects of OPFRs and levels of human exposure. Currently, human biomonitoring data on the levels of OPFR metabolites in the Canadian population are still non-existent. Herein we describe a novel method to measure nine urinary OPFR metabolites using solid phase extraction and ultra performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). The method detection limits were between 0.08 and 0.25ng/mL for target metabolites. The newly developed and validated method was applied to the analysis of 24 urine samples collected in 2010-12 from pregnant Canadian women. The most frequently detected OPFR metabolite in urine of study participants (detection frequency: 97%) was diphenyl phosphate (DPHP), with concentrations ranging between <0.13-25.2ng/mL, followed (75%) by the sum of two metabolites (DoCP: Di-o-cresyl phosphate and DpCP: Di-p- cresyl phosphate) of tricresyl phosphate, with concentrations between <0.13-4.38ng/mL. With the exception of desbutyl-tris-(2-butoxy-ethyl) phosphate which was not detected in any of the samples, all other OPFR metabolites measured were found among study participants with variable detection frequency, suggesting pregnant Canadian women may be exposed to OPFRs.

摘要

在过去几年中,有机磷酸酯阻燃剂(OPFRs)的使用一直在增加;然而,关于OPFRs对人类健康的影响以及人类接触水平方面仍存在知识空白。目前,加拿大人群中OPFR代谢物水平的人体生物监测数据仍然不存在。在此,我们描述了一种使用固相萃取和超高效液相色谱-串联质谱联用(UPLC-MS/MS)来测量九种尿中OPFR代谢物的新方法。目标代谢物的方法检测限在0.08至0.25ng/mL之间。新开发并经过验证的方法应用于对2010 - 2012年从加拿大孕妇中收集的24份尿液样本的分析。研究参与者尿液中最常检测到的OPFR代谢物(检测频率:97%)是磷酸二苯酯(DPHP),浓度范围在<0.13 - 25.2ng/mL之间,其次(75%)是磷酸三甲苯酯的两种代谢物(DoCP:磷酸二邻甲苯酯和DpCP:磷酸二对甲苯酯)之和,浓度在<0.13 - 4.38ng/mL之间。除了在任何样本中均未检测到的磷酸三(2-丁氧基乙基)酯脱丁基代谢物外,所测量的所有其他OPFR代谢物在研究参与者中均有不同的检测频率,这表明加拿大孕妇可能接触到OPFRs。

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