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[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 establish a high performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of 13 phthalate metabolites in human urine. [Method] The urine samples were purified by β-glucuronidase and anion exchange column (Oasis MAX), separated by SB-phenyl RRHD column, detected by electrospray ionization mass spectrometry and quantified by isotope internal standard method. [Results] The 13 metabolites had a good linear relationship in the range of 0.5 ~ 200μg / L, the correlation coefficient was ≥0.999, the detection limit was between 0.1 ~ 0.2μg / L, the recovery was 93.7% ~ 110.3% , Relative standard deviation (RSD) <10%. [Conclusion] The established method for the determination of 13 phthalate metabolites in urine by high performance liquid chromatography-tandem mass spectrometry is suitable for the determination of phthalate metabolites in urine samples and in the population of phthalates Exposure assessment.