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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 XTerraphenyl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 establish a method for the simultaneous determination of 11 phthalate metabolites in urine by liquid chromatography-mass spectrometry / mass spectrometry. Methods The phthalate metabolites in urine samples were hydrolyzed by glucuronidase and enriched with Varian NEXUS solid phase extraction column. The eluted fractions were eluted with methanol / acetonitrile (1: 1, V / V) XTerraphenyl separation, qualitative and quantitative analysis with tandem mass spectrometry in negative ionization mode. Results The detection limits of 11 phthalate metabolites were between 0.13 and 2.27 ng / ml. The recoveries of the two standards were between 67% and 108% with relative standard deviations less than 12%. Conclusion The method for the determination of 11 phthalate metabolites in urine is accurate, reliable and sensitive.