人体尿液中双酚A与壬基酚的同位素稀释的LC-MS/MS分析

采用固相萃取、高效液相色谱-质谱/质谱仪同位素稀释技术,建立了尿中双酚A(BPA)和壬基酚(NP)的检测方法.液相色谱分离用C18柱,流动相为甲醇和水,负离子电喷雾模式电离,多反应离子监测方式检测,BPA和NP的定量离子对分别为m/z 226.9/132.9、219.3/118.8, 13C和氘代同位素化合物分别做回收率控制和内标定量.BPA和NP的基质加标回收率分别为86% ～106%、90% ～114%,定量下限分别为0.97、2.3 μg/L.实际尿样的测定验证了该方法的可行性.

Quantification of Bisphenol A and Nonylphenol in Human Urine by High Performance Liquid Chromatography-Isotope Dilution Tandem Mass Spectrometry

A liquid chromatography coupled to tandem mass spectrometry(LC-MS/MS) method was developed for the determination of urinary bisphenol A(BPA) and nonylphenol(NP) in human urine sample.The cleanup and enrichment of sample was performed by solid-phase extraction.Identification and quantification of BPA and NP were carried out by MS under negative electrospray ionization mode and multiple reaction monitoring(MRM).13C- and D-labelled BPA and NP were used for surrogate recovery and internal standard,and m/z 226.9/132.9,219.3/118.8 were selected as quantification transitions of BPA and NP,respectively.The limits of quantification(LOQ) of BPA and NP were 0.97 μg/L and 2.3 μg/L,respectively.The spiked recoveries of BPA and NP in urine sample were in the range of 86%-106%for BPA and 90%-114%for NP.The developed method was further validated in human urines.