人体尿液中双酚A与壬基酚的同位素稀释的LC-MS/MS分析

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

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、2．3ug／L。实际尿样的测定验证了该方法的可行性。

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 eleetrospray 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 ug/L and 2.3 ug/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.