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On-line coupling of cyclodextrin mediated nonaqueous capillary electrophoresis to mass spectrometry for the determination of salbutamol enantiomers in urine

机译:在线耦合环糊精介导的非水毛细管电泳与质谱法测定尿液中的沙丁胺醇对映体

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摘要

The usefulness of the on-line coupling of nonaqueous capillary electrophoresis (NACE) with electrospray ionization (ESI) mass spectrometry (MS) using heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-cyclodextrin (HDAS-beta-CD) was demonstrated for the enantioselective determination of low concentrations of salbutamol in human urine. After optimization of several parameters, such as sheath-liquid composition and flow rate, nebulizing gas pressure, CE counter-pressure and position of the CE capillary outlet, a limit of quantification of 18 and 20 ng/ml was obtained for salbutamol enantiomers. Moreover, the relative standard deviation values for repeatability at a concentration of 30 ng/ml were below 7% for both enantiomers. Typical regression lines obtained after application of a simple linear regression model revealed a pod relationship between peak area and analyte concentration (with 0.9988 and 0.9966 as coefficients of determination). This paper proposes an easy to use and sensitive NACE-MS method to determine enantiomers of a basic chiral drug in biological fluids preceded by solid-phase extraction as sample cleanup. (c) 2005 Elsevier B.V. All rights reserved.
机译:非水毛细管电泳(NACE)与电喷雾电离(ESI)质谱(MS)在线耦合的有用性,使用七(2,3-二-O-乙酰基-6-O-磺基)-β-环糊精(已证明HDAS-β-CD)可对映测定人尿中低浓度的沙丁胺醇。在优化了几个参数(例如鞘液组成和流速,雾化气体压力,CE反压以及CE毛细管出口的位置)后,沙丁胺醇对映体的定量极限为18和20 ng / ml。而且,两种对映体在浓度为30 ng / ml时,重复性的相对标准偏差值均低于7%。应用简单的线性回归模型后获得的典型回归线显示峰面积与分析物浓度之间具有荚果关系(测定系数为0.9988和0.9966)。本文提出了一种易于使用且灵敏的NACE-MS方法,用于在生物流体中确定基本手性药物的对映体,然后进行固相萃取作为样品净化。 (c)2005 Elsevier B.V.保留所有权利。

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