超高效液相色谱串联质谱同时快速检测环境水体中31种内分泌干扰物

Rapid and simultaneous determination of 31 endocrine disrupting chemicals in aquatic environment by ultra performance liquid chromatography-tandem mass spectrometry

本文建立了固相萃取结合超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)同时测定环境水体中31种内分泌干扰物(EDCs)的分析方法.水样通过MCX固相萃取柱一步富集.采用BEH C_(18)色谱柱(150 mm×2.1 mm i.d.,1.7μm)对化合物进行分离,0.025%氨水-甲醇梯度洗脱,电喷雾正负离子(ESI-、ESI+)两种电离模式切换、多反应监测(MRM)模式进行同时检测,内标法定量.31种EDCs在一定浓度范围内均呈良好的线性关系(R^2≥0.99),方法检出限为0.01—3 ng·L^(-1).对Milli-Q纯水、自来水和地表水进行加标回收,日内、日间相对标准偏差值均小于25%.自来水和地表水样品的平均加标回收率分别为61.2%—150%、54.4%—141%和51.6%—127%、52.2%—143%.此方法一步固相萃取,31种物质同时检测,方便快捷,灵敏度高.该方法成功应用于饮用水和地表水(黄浦江和太湖)中31种EDCs的分析.

A method was developed for the simultaneous determination of 31 endocrine disrupting chemicals（EDCs） in environmental water by solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. Water samples were enriched by MCX solid-phase extraction columns in one step. The separation was performed on a BEH C18column（150 mm×2.1 mm i. d.,1.7 μm） in gradient elution with methanol-0.025% ammonia aqueous solution as the mobile phase. The samples were detected by multiple reaction monitoring（MRM）mode with positive-negative electrospray ionization. Thirty one EDCs were quantified by internal standard method and the calibration curves showed good linearity in a wide range with correlation coefficients（R2） not less than 0.99. The detection limit of EDCs ranged from 0.01—3 ng·L-1. The average recovery of the 31 EDCs spiked in tap water and surface water samples ranged from 61.2%—150%,54.4%—141% and 51. 6%—127%,52. 2%—143% respectively. All the relative standard deviations of EDCs were less than 25%. The developed method is sensitive,convenient,rapid and reliable for the simultaneous determination of 31 EDCs in drinking water and surface water.