Institute of Pharmaceutical Analysis, Interdisciplinary Excellence Centre, University of Szeged, H-6720, Szeged, Somogyi utca 4, Hungary.
Institute of Pharmaceutical Analysis, Interdisciplinary Excellence Centre, University of Szeged, H-6720, Szeged, Somogyi utca 4, Hungary.
J Pharm Biomed Anal. 2021 Jan 30;193:113724. doi: 10.1016/j.jpba.2020.113724. Epub 2020 Oct 29.
In this study, we present results obtained on the diastereo- and enantioseparation of some basic natural and synthetic Cinchona alkaloid analogs by applying liquid chromatographic (LC) and subcritical fluid chromatographic (SFC) modalities on amylose and cellulose tris-(phenylcarbamate)-based stationary phases using n-hexane/alcohol/DEA or CO/alcohol/DEA mobile phase systems. Seven chiral stationary phases in their immobilized form were employed to explore their stereoselectivity for a series of closely related group of analytes. The most important characteristics of LC and SFC systems were evaluated through the variation of the applied chromatographic conditions (e.g., the nature and content of the alcohol modifier, the concentration of additives, temperature). The columns Chiralpak IC and IG turned out to be the best in both LC and SFC modalities. Temperature-dependence study indicated enthalpy-controlled separation in most cases; however, separation controlled by entropy was also registered.
在这项研究中，我们展示了通过应用液相等度洗脱和亚临界流体色谱模式，在手性固定相上对一些基本的天然和合成金鸡纳生物碱类似物进行非对映和对映体拆分的结果。在正己烷/醇/DEA 或 CO/醇/DEA 流动相体系中，使用基于直链淀粉和纤维素三-(苯基氨基甲酸酯)的固定相。我们使用了七种手性固定相的固定化形式来探索它们对一系列密切相关的分析物的立体选择性。通过改变所应用的色谱条件（例如，醇改性剂的性质和含量、添加剂的浓度、温度），评估了 LC 和 SFC 系统的最重要特征。Chiralpak IC 和 IG 柱在 LC 和 SFC 模式下均表现最佳。温度依赖性研究表明，在大多数情况下，分离是由焓控制的；然而，也记录了由熵控制的分离。
