色谱

色谱 ›› 2015, Vol. 33 ›› Issue (6): 622-627.DOI: 10.3724/SP.J.1123.2015.01037

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法同时测定人尿液中7种邻苯二甲酸酯代谢物

高慧1, 许媛媛1,2, 孙丽1, 金忠秀2, 胡海婷1, 盛杰2, 任玲玲2, 陶芳标1,2   

  1. 1. 安徽医科大学公共卫生学院儿少卫生与妇幼保健学系, 安徽 合肥 230032;
    2. 安徽人口健康与优生省级实验室, 安徽 合肥 230032
  • 收稿日期:2015-01-27 出版日期:2015-06-08 发布日期:2015-05-26
  • 通讯作者: 陶芳标
  • 基金资助:

    国家自然科学基金重点项目(81330068);国家自然科学基金青年基金项目(81302449).

Determination of seven phthalate metabolites in human urine by high performance liquid chromatography-tandem mass spectrometry

GAO Hui1, XU Yuanyuan1,2, SUN Li1, JIN Zhongxiu2, HU Haiting1, SHENG Jie2, REN Lingling2, TAO Fangbiao1,2   

  1. 1. Department of Maternal, Child and Adolescent Health, School of Public Health, Anhui Medical University, Hefei 230032, China;
    2. Anhui Provincial Key Laboratory of Population Health & Aristogenics, Hefei 230032, China
  • Received:2015-01-27 Online:2015-06-08 Published:2015-05-26

PDF

391

被引次数

13

摘要：

建立了同时检测人尿液中7种邻苯二甲酸酯代谢物的高效液相色谱-串联三重四极杆质谱法。尿液经酶水解后,采用萃取柱净化,以2%(v/v)甲酸甲醇溶液为洗脱剂,经苯基柱分离,以0.1%(v/v)乙酸水溶液和0.1%(v/v)乙酸乙腈溶液为流动相进行梯度洗脱,采用电喷雾离子源负离子模式和多反应监测模式采集信号,用同位素内标法进行定量分析。尿液中7种邻苯二甲酸酯代谢物在0.2~200.0 μg/L范围内定量离子的相对峰面积比值与质量浓度均呈良好线性关系(r≥0.99976);检出限(LOD)为13.43~80.21 ng/L,定量限为44.77~267.37 ng/L; 3个水平的加标回收率为88.8%~108.9%,日内和日间精密度均不大于17.05%。该方法可同时准确、灵敏、简便地测定人尿液中7种邻苯二甲酸酯代谢物的暴露水平。

关键词: 高效液相色谱-串联质谱, 固相萃取, 邻苯二甲酸酯代谢物, 尿, 同位素内标法

Abstract:

A method has been developed for the analysis of seven metabolites of phthalates in human urine by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The urine samples were hydrolyzed with glucuronidase followed by purification with solid-phase extraction (SPE) cartridges. Both 0.1% formic acid in water (v/v) and 0.1% formic acid in acetonitrile were used as the mobile phases in a gradient mode. The chromatographic separation was achieved on a phenyl column. Mass detection was then conducted by electrospray ionization in negative ion mode and multiple reaction monitoring mode. The components were quantified by stable isotope-labelled (13C-) phthalate monoester internal standards. The calibration curves of the seven phthalates metabolites showed good linear relationships in the range of 0.2-200.0 μg/L (r>0.99976). The recoveries at three levels were from 88.8% to 108.9% with relative standard deviations no more than 17.05%. The limits of detection of the method were 13.43-80.2 ng/L. The limits of quantification were 44.77-267.37 ng/L. This method was successfully applied to the determination of metabolism of phthalates in human urine with efficiency, increased accuracy and high sensitivity.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), isotope internal standard method, phthalate metabolites, solid-phase extraction (SPE), urine

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