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0.2~200.0μg／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。
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% for-mic acid in acetonitrile were used as the mobile phases in a gradient mode. The chromatograph-ic separation was achieved on a phenyl column. Mass detection was then conducted by electros-pray ionization in negative ion mode and multiple reaction monitoring mode. The components were quantified by stable isotope-labelled( 13 C-)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.
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