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 Chromatography-Tandem Mass Spectrometry

[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0.5-200μg/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0.1-0.2μg/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。

[ 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-glueuronidase 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 200 μg/L with the correlation coefficients above 0.999 for all tested 13 metabolites. The limits of detection were between 0.1 μg/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.