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 C18色谱柱(150 mm×2.1 mmi.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(R2≥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 C18 column (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.
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