Gao Hui, Xu Yuanyuan, Sun Li, Jin Zhongxiu, Hu Haiting, Sheng Jie, Ren Lingling, Tao Fangbiao
Se Pu. 2015 Jun;33(6):622-7. doi: 10.3724/sp.j.1123.2015.01037.
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 > 0.999 76). 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.
已开发出一种通过高效液相色谱 - 串联质谱法（HPLC-MS/MS）分析人尿中七种邻苯二甲酸酯代谢物的方法。尿样先用葡萄糖醛酸酶水解，然后用固相萃取（SPE）柱进行纯化。水（v/v）中的0.1%甲酸和乙腈中的0.1%甲酸均用作梯度模式下的流动相。在苯基柱上实现色谱分离。然后通过电喷雾电离在负离子模式和多反应监测模式下进行质谱检测。各组分通过稳定同位素标记（13C-）邻苯二甲酸单酯内标进行定量。七种邻苯二甲酸酯代谢物的校准曲线在0.2 - 200.0 µg/L范围内呈良好线性关系（r > 0.999 76）。三个加标水平的回收率为88.8%至108.9%，相对标准偏差不超过17.05%。该方法的检测限为13.43 - 80.2 ng/L。定量限为44.77 - 267.37 ng/L。该方法已成功应用于人尿中邻苯二甲酸酯代谢物的测定，具有高效、准确性提高和高灵敏度的特点。
