朱效宁, 汪国权, 周志俊, 卢大胜, 邬春华, 方红, 严玉洁, 金玉娥. 尿中13种邻苯二甲酸酯代谢物的高效液相色谱串联质谱测定法[J]. 环境与职业医学, 2015, 32(3): 265-270. DOI: 10.13213/j.cnki.jeom.2015.14234
引用本文: 朱效宁, 汪国权, 周志俊, 卢大胜, 邬春华, 方红, 严玉洁, 金玉娥. 尿中13种邻苯二甲酸酯代谢物的高效液相色谱串联质谱测定法[J]. 环境与职业医学, 2015, 32(3): 265-270. DOI: 10.13213/j.cnki.jeom.2015.14234
ZHU Xiao-ning , WANG Guo-quan , ZHOU Zhi-jun , LU Da-sheng , WU Chun-hua , FANG Hong , YAN Yu-jie , JIN Yu-e . Detecting 13 Phthalate Metabolites in Human Urine by High Performance Liquid ChromatographyTandem Mass Spectrometry[J]. Journal of Environmental and Occupational Medicine, 2015, 32(3): 265-270. DOI: 10.13213/j.cnki.jeom.2015.14234
Citation: ZHU Xiao-ning , WANG Guo-quan , ZHOU Zhi-jun , LU Da-sheng , WU Chun-hua , FANG Hong , YAN Yu-jie , JIN Yu-e . Detecting 13 Phthalate Metabolites in Human Urine by High Performance Liquid ChromatographyTandem Mass Spectrometry[J]. Journal of Environmental and Occupational Medicine, 2015, 32(3): 265-270. DOI: 10.13213/j.cnki.jeom.2015.14234

尿中13种邻苯二甲酸酯代谢物的高效液相色谱串联质谱测定法

Detecting 13 Phthalate Metabolites in Human Urine by High Performance Liquid ChromatographyTandem Mass Spectrometry

  • 摘要: 目的 建立同时测定人尿中13种邻苯二甲酸酯代谢物的高效液相色谱-串联质谱法。

    方法 尿样经β-葡萄糖苷酸酶水解、阴离子交换固相萃取柱(Oasis MAX)净化后,经SB-phenyl RRHD柱分离,电喷雾电离质谱检测,同位素内标法定量。

    结果 13种代谢物在0.5~200 μg/L的范围内均具有良好的线性关系,相关系数均 ≥ 0.999,检出限在0.1~0.2 μg/L之间,回收率为93.7%~110.3%,相对标准偏差(RSD)均 < 10%。

    结论 建立的检测尿中13种邻苯二甲酸酯代谢物的高效液相色谱串联质谱法适用于尿样中邻苯二甲酸酯代谢物的含量测定和人群邻苯二甲酸酯暴露评估。

     

    Abstract: Objective To develop a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for simultaneously determining 13 phthalate metabolites in human urine.

    Methods Urine samples were prepared by hydrolyzation with beta-glucuronidase and extraction by solid-phase extraction, and then separated on a SB-phenyl RRHD column before applying isotope dilution-HPLC-MS/MS.

    Results Good linear relationships were obtained in the range of 0.5 μg/L to 200μg/L with the correlation coefficients above 0.999 for all tested 13 metabolites. The limits of detection were between 0.1μg/L and 0.2 μg/L. The recoveries were in the range of 93.7% to 110.3%, and all relative standard deviations (RSD) were lower than 10%.

    Conclusion A sensitive analytical method, based on SPE followed by isotope dilution-HPLC-MS/MS, to quantitatively measure 13 phthalate metabolites in human urine has been developed and validated.

     

/

返回文章
返回