彭凡立, 吉文亮, 彭丹红, 朱峰, 杨淼, 刘冉, 浦跃朴, 尹立红. 超高效液相色谱串联质谱检测尿液中6种环境内分泌干扰物方法的建立与应用[J]. 环境与职业医学, 2016, 33(5): 499-503. DOI: 10.13213/j.cnki.jeom.2016.15717
引用本文: 彭凡立, 吉文亮, 彭丹红, 朱峰, 杨淼, 刘冉, 浦跃朴, 尹立红. 超高效液相色谱串联质谱检测尿液中6种环境内分泌干扰物方法的建立与应用[J]. 环境与职业医学, 2016, 33(5): 499-503. DOI: 10.13213/j.cnki.jeom.2016.15717
PENG Fan-li, JI Wenliang, PENG Dan-hong, ZHU Feng, YANG Miao, LIU Ran, PU Yue-pu, YIN Li-hong. Establishment and Application of Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Detecting Six Environmental Endocrine Disruptors in Urine[J]. Journal of Environmental and Occupational Medicine, 2016, 33(5): 499-503. DOI: 10.13213/j.cnki.jeom.2016.15717
Citation: PENG Fan-li, JI Wenliang, PENG Dan-hong, ZHU Feng, YANG Miao, LIU Ran, PU Yue-pu, YIN Li-hong. Establishment and Application of Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Detecting Six Environmental Endocrine Disruptors in Urine[J]. Journal of Environmental and Occupational Medicine, 2016, 33(5): 499-503. DOI: 10.13213/j.cnki.jeom.2016.15717

超高效液相色谱串联质谱检测尿液中6种环境内分泌干扰物方法的建立与应用

Establishment and Application of Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Detecting Six Environmental Endocrine Disruptors in Urine

  • 摘要: 目的

    建立超高效液相色谱串联质谱(UPLC-MS/MS)检测人尿液中4种塑化剂代谢产物、双酚A(BPA)和壬基酚(NP)含量的方法,分析南京地区育龄期妇女对6种典型环境内分泌干扰物的暴露水平。

    方法

    建立针对塑化剂代谢产物、BPA和NP的尿液样品前处理方法以及UPLC-MS/MS检测方法,考察方法的回收率和日内、日间精密度。用所建立的方法对南京地区120份育龄期妇女尿液样品中塑化剂代谢产物、BPA和4-n-NP进行定量分析。

    结果

    4种塑化剂代谢产物、BPA和4-n-NP在1~100 μg/L范围内均线性关系良好(r2>0.998),其中邻苯二甲酸单正丁酯(MBP)、邻苯二甲酸单异丁酯(MiBP)、邻苯二甲酸单苄酯(MBzP)和邻苯二甲酸单(2-乙基)己酯(MEHP)检测限均为0.1 μg/L。BPA和4-n-NP检测限为0.3 μg/L。固相萃取回收率均在92.3%~103.5%,日间及日内精密度均小于10%。育龄期妇女尿液中MBP、MiBP、MBzP、MEHP、BPA和4-n-NP质量浓度中位数分别为5.04、2.10、0.42、5.24、1.32和1.47 μg/L。

    结论

    本研究建立的尿液中塑化剂代谢产物、BPA和4-n-NP检测方法具有灵敏度高、定量准确的优势。南京地区育龄期妇女尿液中MBP、MiBP、MBzP、MEHP和BPA有较高检出率。

     

    Abstract: Objective

    To establish a method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to assess six kinds of environmental endocrine disruptors including four phthalate metabolites (MPAEs), bisphenol A (BPA), and nonylphenol (NP) in the urine of women of reproductive age in Nanjing.

    Methods

    Pretreatment and UPLCMS/MS analytical method was established for MPAEs, BPA, and NP. The accuracy, intra-day precision, and inter-day precision of the method were assessed. Then 120 urine samples collected from women of reproductive age in Nanjing were measured for concentrations of phthalate metabolites, BPA, and 4-n-NP.

    Results

    All the analytes were linear over the range of 1-100 μg/L (r2>0.998). The limits of detection were 0.1 μg/L for mono-n-butyl phthalate (MBP),mono-isobutyl phthalate (MiBP), mono-benzyl phthalate (MBzP), and mono-2-ethylhexyl phthalate (MEHP), and 0.3 μg/L for BPA and 4-n-NP. The recoveries by solid phase extraction of all analytes ranged from 92.3% to 103.5%; the intra-day and inter-day precisions were all less than 10%. The median concentrations of MBP, MiBP, MBzP, MEHP, BPA, and 4-n-NP were 5.04, 2.10, 0.42, 5.24, 1.32, and 1.47 μg/L, respectively.

    Conclusion

    The sensitive and accurate method is suitable for the determination of MPAEs, BPA and 4-n-NP in urine. Women of reproductive age present high positive rates of MBP, MiBP, MBzP, MEHP, and BPA.

     

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