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首页> 外文会议>NATO Advanced Study Institute on Chemicals as Intentional and Accidental Global Environmental Threats >METHOD FOR THE DETERMINATION OF SOME SELECTED STEROID HORMONES AND BISPHENOL A IN WATER AT LOW NG/L LEVEL BY ON-LINE SOLID-PHASE EXTRACTION COMBINED WITH LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY
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METHOD FOR THE DETERMINATION OF SOME SELECTED STEROID HORMONES AND BISPHENOL A IN WATER AT LOW NG/L LEVEL BY ON-LINE SOLID-PHASE EXTRACTION COMBINED WITH LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

机译：通过在线固相萃取与液相色谱 - 串联质谱结合在低Ng / L水平下测定一些选定类固醇激素和水在水中的双酚A.

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A sensitive analytical method based on automatic on-line Solid-Phase Extraction (SPE) combined with Liquid Chromatography-Tandem Mass Spectrometry (LC-ESI-MS-MS) has been developed for the determination of six Endocrine-Disrupting Compounds (EDC's): 17-α-estradiol, 17-α-ethynylestradiol, 17-β-estradiol, bisphenol A, Estriol and Estrone in water samples. In order to enhance the sensitivity for these analytes, post column addition of different bases such as ammonia and 1,8-diazabicyclo(5,4,0)undec-7en (DBU) was evaluated. The post column addition of base is proposed here to raise effluent pH, helping in the ionization process of the compounds. The use of ammonium hydroxide diluted in methanol-acetonitrile mixture, proved to be the most efficient post column reagent for enhancing the MS signal. This strategy permitted direct determination of the six compounds at low ng/L levels. For the application to real water samples, an extraction and preconcentration step using SPE was carried out with cross-linked styrene-divinylbenzene polymer (PLPR-s) material. The recovery for all six compounds was satisfactory percentage (80-110%). The limits of quantification are between 1.0 and 2.0 ng/L. Application of the whole method, SPE-LC-ESI-MS-MS, to nature waters permitted low nanogram-per-liter determination of all six compounds.
机译：已经开发了一种基于自动在线固相萃取（SPE）与液相色谱 - 串联质谱（LC-ESI-MS-MS）组合的敏感性分析方法用于测定六个内分泌破坏化合物（EDC）： 17-α-雌二醇，17-α-乙炔雌二醇，17-β-雌二醇，双酚A，雌醇和水样中的雌激素。为了增强这些分析物的敏感性，评价柱柱添加不同碱，例如氨和1,8-二氮杂双环（5,4,0）UNDEC-7EN（DBU）。提出了柱中加入碱以提高流出物pH，帮助化合物的电离过程。在甲醇 - 乙腈混合物中稀释的氢氧化铵的用途证明是最有效的柱柱试剂，用于增强MS信号。该策略允许直接测定低Ng / L水平的六种化合物。对于真实水样的施用，使用SPE的提取和前浓缩步骤用交联的苯乙烯 - 二乙烯基苯聚合物（PLPR-S）材料进行。所有六种化合物的恢复令人满意的百分比（80-110％）。定量限介于1.0和2.0 ng / L之间。整个方法的应用，SPE-LC-ESI-MS-MS，对自然水允许低纳米每升所有六种化合物的测定。

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