Determination of Phenolic Endocrine Disrupting Chemicals in Human Urine by High Performance Liquid Chromatography Tandem Electrospray Ionization Mass Spectrometry

采用通用电喷雾离子源的高效液相色谱-串联质谱(HPlC-ESI MS/MS)分析技术,通过丹磺酰氯衍生化处理,建立了同时测定人尿液中双酚A(bPA)、三氯生(TCS)、炔雌酮(EE2)、雌酮(E1)、雌二醇(E2)5种酚类内分泌干扰物的高灵敏方法。5种酚类化合物在0.2~100μg/l质量浓度范围内线性关系良好,相关系数(r2)均在0.99以上,检出限(lOd)在0.02~0.27μg/l之间。在5、10、50μg/l加标水平下,平均回收率为85%~125%,相对标准偏差(rSd,n=3)为0.53%~14.4%。该方法灵敏度高、重现性好、回收率高、操作简单,可作为人尿液中酚类内分泌干扰物暴露分析的备选方法之一。A high performance liquid chromatography tandem electrospray ionization mass spectrometry(HPLC-ESI MS/MS) method was developed and validated for the determination of phenolic endocrine disrupting chemicals(EDCs),including bisphenol A(BPA),triclosan(TCS),17α-ethynylestradiol(EE2),estrone(E1) and 17 β-estradiol(E2)in human urine.The samples were purified by liquid-liquid extraction,derivertized with dansyl chloride,and detected by HPLC-ESI MS/MS.The target compounds were quantified by the stable isotope dilution technique.The calibration curve were linear in the range of 0.2-100 μg/L for the 5 EDCs with correlation coefficients more than 0.99.The limits of detection of 5 EDCs were in the range of 0.02-0.27 μg/L.The matrix recoveries of the method for 5 EDCs at three spiked levels of 5,10 and 50 μg/L ranged from 85% to 125%.The relative standard deviations(RSDs,n=3) were between 0.53% and 14.4%.The method was successfully applied in the analysis of 5 EDCs in human urine with its sensitivity and accurancy.中科院“百人计划”项目; 厦门市科技计划项目(3502Z20122003