Kot A, Sandra P, Venema A
Department of Organic Chemistry, University of Ghent, Belgium.
J Chromatogr Sci. 1994 Oct;32(10):439-48. doi: 10.1093/chromsci/32.10.439.
Various chiral stationary phases were investigated in sub- and supercritical fluid chromatography for the separation, without derivatization, of basic (beta-blockers, benzodiazepines) and acidic (nonsteroidal anti-inflammatory drugs, beta-agonists) pharmaca. For all racemates, baseline separation was achieved within short analysis times. For several solutes, the high resolution obtained allowed injection of milligram amounts and semipreparative collection of the enantiomers. The parameters affecting enantioselectivity (column efficiency, influence of modifiers and basic or acidic additives, and temperature) have been studied. Enantiomerization of 3-OH-benzodiazepines could be suppressed by working at low temperatures or by using acetonitrile as a comodifier. Serial coupling of different chiral stationary phase columns resulted in a column triplet (Chiralpak AD, an amylose derivative; Chiralcel OD, a cellulose derivative; and Chirex 3022, a Brush-type with pi-donor characteristics) on which all solutes investigated could be baseline separated.
在亚临界和超临界流体色谱中研究了各种手性固定相，用于在不衍生化的情况下分离碱性（β-受体阻滞剂、苯二氮䓬类）和酸性（非甾体抗炎药、β-激动剂）药物。对于所有外消旋体，在短分析时间内实现了基线分离。对于几种溶质，所获得的高分辨率允许进样毫克量并对映体进行半制备收集。研究了影响对映体选择性的参数（柱效、改性剂以及碱性或酸性添加剂的影响和温度）。通过在低温下操作或使用乙腈作为共改性剂，可以抑制3-OH-苯二氮䓬类的对映异构化。不同手性固定相柱的串联耦合产生了一个三联柱（Chiralpak AD，一种直链淀粉衍生物；Chiralcel OD，一种纤维素衍生物；以及Chirex 3022，一种具有π-供体特性的刷型柱），在所研究的所有溶质上都可以实现基线分离。
