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手性固定相在超临界流体色谱中拆分药物对映异构体。

Pharmaceutical-enantiomers resolution using immobilized polysaccharide-based chiral stationary phases in supercritical fluid chromatography.

机构信息

Department of Analytical Chemistry and Pharmaceutical Technology (FABI), Center for Pharmaceutical Research (CePhaR), Vrije Universiteit Brussel - VUB, Laarbeeklaan 103, B-1090 Brussels, Belgium.

Department of Analytical Chemistry and Pharmaceutical Technology (FABI), Center for Pharmaceutical Research (CePhaR), Vrije Universiteit Brussel - VUB, Laarbeeklaan 103, B-1090 Brussels, Belgium.

出版信息

J Chromatogr A. 2014 Feb 7;1328:85-97. doi: 10.1016/j.chroma.2013.12.044. Epub 2014 Jan 7.

Abstract

Since their introduction on the market the applicability of immobilized polysaccharide-based chiral stationary phases in high-performance liquid chromatography has been thoroughly investigated. These immobilized phases have the benefit to be applicable with a wide range of modifiers, potentially extending the application range of the polysaccharide-based stationary phases. Because an increasing number of stationary phases are being introduced in the field of chiral chromatography it is important to evaluate their enantioselectivity in different techniques in order to get an idea about their applicability. In this study, three immobilized chiral polysaccharide-based stationary phases (Chiralpak IA, IB, and IC) are evaluated in supercritical fluid chromatography (SFC) with a test set of pharmaceutical racemates. This is done in a three-fold manner: their performance is evaluated (1) using traditional modifiers, (2) using mixtures of atypical modifiers, and (3) the results were compared to those on coated stationary phases with an equivalent chiral selector. To get a visual overview of the enantioselective patterns of the different chromatographic systems (mobile and stationary phase combinations), a Principal Component Analysis is performed, which allows determining the (dis)similarity between individual systems. To assess the complementarity cumulative success rates are determined. The immobilized chiral stationary phases prove to yield high cumulative success rates.

摘要

自上市以来,固定化多糖手性固定相在高效液相色谱中的适用性已经得到了深入研究。这些固定相的优点是可以与多种改性剂一起使用,从而潜在地扩展多糖手性固定相的应用范围。由于手性色谱领域中引入了越来越多的固定相,因此评估它们在不同技术中的对映选择性以了解它们的适用性非常重要。在这项研究中,使用一组药物外消旋体,在超临界流体色谱(SFC)中评估了三种固定化手性多糖固定相(Chiralpak IA、IB 和 IC)。这是通过三种方式进行的:(1)使用传统改性剂评估它们的性能,(2)使用非典型改性剂混合物评估它们的性能,(3)将结果与具有等效手性选择器的涂层固定相的结果进行比较。为了直观地了解不同色谱系统(流动相和固定相组合)的对映选择性模式,进行了主成分分析,该分析允许确定各个系统之间的(不)相似性。为了评估互补性,确定了累积成功率。固定化手性固定相证明可以获得高的累积成功率。

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