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评价超临界流体色谱中用于改善对映异构体拆分的固定相手性选择剂的非常规极性修饰。

Evaluation of non-conventional polar modifiers on immobilized chiral stationary phases for improved resolution of enantiomers by supercritical fluid chromatography.

机构信息

Merck Research Laboratories, Rahway, NJ 07065, USA.

Merck Research Laboratories, Rahway, NJ 07065, USA.

出版信息

J Chromatogr A. 2014 Feb 7;1328:98-103. doi: 10.1016/j.chroma.2013.12.073. Epub 2013 Dec 31.

Abstract

An evaluation of the use of non-conventional polar modifiers for the supercritical fluid chromatographic separation of enantiomers on immobilized chiral stationary phases is presented. The resolution of a group of nine commercially available racemates is studied on the Chiralpak IA, IB, IC, ID, IE, and IF chiral stationary phases using CO2-based eluents containing non-conventional polar modifiers such as dichloromethane, chloroform, tetrahydrofuran, 2-methyl tetrahydrofuran, methyl tert-butyl ether, cyclopentyl methyl ether, acetone, ethyl acetate, toluene, 2,2,2-trifluoroethanol, and N,N-dimethylformamide. Screening experiments and method development for the commercial racemates on the immobilized columns with the non-conventional solvents demonstrated an ability to adjust the retention and improve resolution. From these results we were able to assign a general eluotropic relationship between the non-conventional solvents and methanol. A general ability to selectively adjust chromatographic retention while improving analyte solubility can lead to improved preparative chromatographic performance.

摘要

本文评价了在固定相手性柱上使用超临界流体色谱拆分对映异构体时,非传统极性改性剂的应用。使用基于 CO2 的洗脱剂,其中包含二氯甲烷、氯仿、四氢呋喃、2-甲基四氢呋喃、甲基叔丁基醚、环戊基甲基醚、丙酮、乙酸乙酯、甲苯、2,2,2-三氟乙醇和 N,N-二甲基甲酰胺等非传统极性改性剂,研究了一组 9 种市售外消旋体在 Chiralpak IA、IB、IC、ID、IE 和 IF 手性固定相上的分离情况。通过在固定柱上使用非传统溶剂进行筛选实验和方法开发,证明了能够调节保留时间并提高分辨率。根据这些结果,我们能够确定非传统溶剂与甲醇之间的一般洗脱关系。通常能够选择性地调节色谱保留时间,同时提高分析物的溶解度,可以提高制备色谱的性能。

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