超高效液相色谱-串联质谱法检测饮用水中8种激素的含量及污染状况  

Determination of 8 hormones concentrations in drinking water by ultra performance liquid chromatography-tandem mass spectrometry and its contamination

作　　者：徐淑暖[1] 张少彬[1] 张文改[1] 陈砚朦[1] 林晓燕 任园园 

机构地区：[1]东莞市疾病预防控制中心,广东东莞523000

出　　处：《中国卫生检验杂志》2017年第20期2900-2904,2913,共6页Chinese Journal of Health Laboratory Technology

基　　金：东莞市科技计划医疗卫生类科研项目(2015105150-00765)

摘　　要：目的建立饮用水中的雌酮(E1)、17β-雌二醇(E2)、17α-炔雌醇(EE2)、雌三醇(E3)、双烯雌酚(DE)、己烯雌酚(DES)、双酚A(BPA)和4-叔辛基苯酚(4-OP)的超高效液相色谱-串联质谱检测方法,并用于东莞市饮用水中8种激素的含量检测和评价。方法水样经固相萃取净化后,采用UPLC-ESI-MS/MS、负离子方式、多离子反应监测(MRM)定量,对东莞市市级及镇区各水厂水源水、出厂水、直饮水及反渗透水中8种激素的含量进行检测。结果 8种激素在1.0μg/L^100μg/L浓度时有良好的线性关系,方法的检出限为0.000 3μg/kg,平均回收率为75.0%~118.0%,相对标准偏差为4.0%~11.0%。结论建立的方法准确可行,用于饮用水中8种激素的检测,部分饮用水检出双酚A和4-叔辛基苯酚。Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-ESI-MS/MS） method for the determination of 8 hormones,including estrone（ E1）,17β-estradiol（ E2）,17α-ethinyloestradiol（ EE2）,estriol（ E3）,dienestrol（ DE）,diethylstilbestrol（ DES）,bisphenol-A（ BPA）,4-tertbutylphenol（ 4-OP） in drinking water,and to perform it in the contamination levels detection and evaluation of 8 hormones in drinking water in Dongguan.Methods Water samples including source water,treated water,direct drinking water and reverse osmosis water from downtowns and towns of Dongguan were pretreated by solid phase extraction（ SPE） and centrifugation. The hormones were analyzed by UPLC-ESI-MS/MS with negative electrospray ionization and multiple-reaction monitoring. Results Good linearities were obtained when the concentrations of the 8 hormones were within 1. 0 μg/L-100. 0 μg/L. The limit of detection was 0. 000 3 μg/kg.The average recoveries were within 75. 0%-118. 0%,and relative standard deviation（ RSD） was within 4. 0%-11. 0%.Conclusion The method is accurate and reliable,which can be used to detect the 8 hormones in the drinking water. BPA and4-OP are detected in some samples.

关 键 词：超高效液相色谱-串联质谱法 固相萃取 饮用水 激素 

分 类 号：R123.1[医药卫生—环境卫生学]