Department of Analytical Chemistry and Pharmaceutical Technology (FABI), Center for Pharmaceutical Research (CePhaR), Vrije Universiteit Brussel - VUB, Laarbeeklaan 103, B-1090 Brussels, Belgium.
J Chromatogr A. 2012 Dec 21;1269:336-45. doi: 10.1016/j.chroma.2012.07.090. Epub 2012 Aug 4.
The enantioselectivity of twelve chiral stationary phases (CSPs) and four methanol-containing carbon dioxide mobile phases (MPs) is evaluated in supercritical fluid chromatography (SFC) with a test set of 59 chiral pharmaceutical compounds. Methanol (MeOH) is evaluated as modifier in carbon dioxide (CO(2)) since it is commonly used in chiral SFC because of its favorable characteristics and proven successes. In addition to the MP of earlier defined generic screening conditions, new MPs, which contained both a basic (isopropylamine) and an acidic (trifluoroacetic acid) additive, were investigated and yielded broad enantioselectivities. The joint use of the additives impacts the enantioselectivity differently than the individual. Polysaccharide-based CSPs from different manufacturers were assessed, which showed that CSPs containing the same selector do not always display the same enantioselectivity. This work enabled not only to identify the individual chiral systems with the broadest enantioselectivity but also to determine their complementarity, resulting in a limited set of systems with the broadest enantioselectivity. As a result an updated, fast and efficient screening sequence was proposed.
评估了十二种手性固定相(CSP)和四种含甲醇的二氧化碳流动相(MP)在超临界流体色谱(SFC)中的对映选择性,使用了 59 种手性药物化合物的测试集。甲醇(MeOH)作为二氧化碳(CO2)中的改性剂进行评估,因为由于其良好的特性和成功经验,甲醇在手性 SFC 中被广泛使用。除了之前定义的通用筛选条件的 MP 外,还研究了新的 MP,其中包含碱性(异丙胺)和酸性(三氟乙酸)添加剂,结果显示出广泛的对映选择性。添加剂的联合使用对映选择性的影响与单独使用添加剂不同。评估了来自不同制造商的基于多糖的 CSP,结果表明,即使 CSP 中含有相同的选择器,它们也不一定具有相同的对映选择性。这项工作不仅能够识别具有最广泛对映选择性的各个手性体系,还能够确定它们的互补性,从而得到一组具有最广泛对映选择性的有限体系。因此,提出了一种更新、快速和有效的筛选序列。