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Simultaneous achiral-chiral analysis of pharmaceutical compounds using two-dimensional reversed phase liquid chromatography-supercritical fluid chromatography

机译:二维反相液相色谱-超临界流体色谱法同时进行非手性手性分析

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摘要

A new interface was designed to enable the coupling of reversed phase liquid chromatography (RPLC) and supercritical fluid chromatography (SFC). This online two-dimensional chromatographic system utilizing RPLC in the first dimension and SFC in the second was developed to achieve simultaneous achiral and chiral analysis of pharmaceutical compounds. The interface consists of an eight-port, dual-position switching valve with small volume C-18 trapping columns. The peaks of interest eluting from the first RPLC dimension column were effectively focused as sharp concentration pulses on small volume C-18 trapping columnis and then injected onto the second dimension SFC column. The first dimension RPLC separation provides the achiral purity result, and the second dimension SFC separation provides the chiral purity result (enantiomeric excess). The results are quantitative enabling simultaneous achiral, chiral analysis of compounds. The interface design and proof of concept demonstration are presented. Additionally, comparative studies to conventional SFC and case studies of the applications of 2D LC-SFC in pharmaceutical analysis is presented. (C) 2015 Elsevier B.V. All rights reserved.
机译:设计了一个新接口,以实现反相液相色谱(RPLC)和超临界流体色谱(SFC)的耦合。该在线二维色谱系统是在第一维中使用RPLC并在第二维中使用SFC进行开发的,以实现对药物化合物的非手性和手性分析。该接口由一个带小容量C-18捕集柱的八通双位切换阀组成。从第一个RPLC尺寸色谱柱洗脱的目标峰以尖锐的浓度脉冲有效聚焦在小体积C-18捕集色谱柱上,然后注入第二维SFC色谱柱。第一维RPLC分离可提供非手性纯度的结果,第二维SFC分离可提供手性纯度的结果(对映体过量)。结果是定量的,能够同时进行化合物的非手性手性分析。介绍了界面设计和概念验证演示。此外,还介绍了与常规SFC的对比研究以及2D LC-SFC在药物分析中的应用案例研究。 (C)2015 Elsevier B.V.保留所有权利。

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