液相色谱-质谱/质谱法测定尿中11种邻苯二甲酸酯代谢物

Simultaneous determination of 11 phthalate metabolites in urine by liquid chromatography tandem mass spectrometry

目的建立同时测定尿中11种邻苯二甲酸酯代谢物的液相色谱-质谱/质谱的方法。方法尿样中邻苯二甲酸酯代谢物经葡萄糖苷酸酶水解后,采用瓦里安NEXUS固相萃取柱富集,甲醇/乙腈（1∶1,V/V）洗脱后,经Waters XTerraphenyl分离,在负电离模式下用串联质谱仪定性定量分析。结果 11种邻苯二甲酸酯代谢物的方法检出限为0.13～2.27ng/ml,两个水平的加标回收率在67%～108%,相对标准偏差均小于12%。结论该方法测定尿中11种邻苯二甲酸酯代谢物方法准确可靠,灵敏度高。

Objective To develop a method for determining 11 kinds of phthalate metabolites in urine simultaneously.Methods The phthalate metabolites in human urine samples were hydrolyzed by glucuronidase,and then were concentrated by solid-phase extraction and eluted by methanol/acetonitrile（1∶1,V/V）.After chromatographic separation on phenyl column,the analytes were analyzed qualitatively and quantitatively under MRM mode.Results The limits of detection（LOD） for the eleven kinds of phthalate metabolites were in the range of 0.13-2.27 ng/ml.The mean recoveries at the two spiked levels were 67%-108%,with the relative standard deviation（RSD） of less than 12%.Conclusion The method can be used to determine the residues of eleven kinds of phthalate metabolites in urine accurately and sensitively.