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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >On-line solid-phase extraction with on-support derivatization for high-sensitivity liquid chromatography tandem mass spectrometry of estrogens in influent/effluent of wastewater treatment plants
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On-line solid-phase extraction with on-support derivatization for high-sensitivity liquid chromatography tandem mass spectrometry of estrogens in influent/effluent of wastewater treatment plants

机译：在线固相萃取-支持衍生化技术用于废水处理厂进水/流出液中高灵敏度液相色谱串联质谱法中的雌激素

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A solid-phase extraction coupled to liquid chromatography/tandem mass spectrometry for the determination of estrogens in sewage influent and effluent has been performed. The possibility of preparing estrogen derivatives directly on a solid-phase extraction bed in which the targeted analytes have been previously isolated and pre-concentrated was explored. This method uses an Oasis HLB column (2.1 mm x 20 mm i.d.) for on-line sample cleanup and derivatization support, and a Sunfire C-18 column (150 mm x 2.1 mm i.d.) with a mobile phase consisting of acetonitrile-water-formic acid for separation. After sample introduction, some matrix interferences are removed by washing up SPE column with methanol-water. Phenolic hydroxyl group of estrogens is subsequently derivatized with dansyl chloride. Reaction takes place in the on-line solid-phase extraction column. The excess of reagent and other matrix interferences are then removed by a second washing. Dansylated estrogens are further back eluted and analyzed with HPLC-MS-MS. The optimized on-line protocol is emphasized owing to a low limit of quantification (1 ng L-1) is achieved with only around 1 mL of sample and a low sensitive MS instrument. Developed strategy has been demonstrated to be an improvement over existing methods due to its greater sensitivity and the low volume of matrix used and the total analysis time (extraction, derivatization, analysis) is less than 17 min. (c) 2007 Elsevier B.V. All rights reserved.
机译：进行了固相萃取-液相色谱/串联质谱联用测定污水进水和出水中的雌激素。探索了直接在固相萃取床上制备雌激素衍生物的可能性，在固相萃取床上先前已分离并预浓缩了目标分析物。该方法使用Oasis HLB色谱柱（2.1 mm x 20 mm内径）进行在线样品净化和衍生化支持，使用Sunfire C-18色谱柱（150 mm x 2.1 mm内径）流动相由乙腈-水-用于分离甲酸。样品引入后，通过用甲醇-水洗涤SPE色谱柱除去一些基质干扰物。随后用丹磺酰氯衍生化雌激素的酚羟基。反应在在线固相萃取塔中进行。然后通过第二次洗涤除去过量的试剂和其他基质干扰物。进一步反洗脱丹磺酰化的雌激素，并用HPLC-MS-MS分析。由于仅使用约1 mL样品和低灵敏度MS仪器即可实现低定量限（1 ng L-1），因此强调了优化的在线方案。由于其较高的灵敏度和所用基质的体积小，并且总分析时间（提取，衍生化，分析）少于17分钟，因此已证明开发的策略是对现有方法的改进。 （c）2007 Elsevier B.V.保留所有权利。

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