Department of Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research, Vrije Universiteit Brussel-VUB, Laarbeeklaan 103, B-1090 Brussels, Belgium.
J Pharm Biomed Anal. 2013 Mar 5;75:74-85. doi: 10.1016/j.jpba.2012.11.019. Epub 2012 Nov 23.
Nine polysaccharide-based chiral stationary phases (CSPs) were used to define a separation strategy that combines normal-phase (NP), reversed-phase (RP) and polar organic solvent chromatography (POSC) modes. After limiting ourselves to two CSPs per mode, in total, five CSPs, Chiralpak AD (NP), Chiralcel OD (RP and POSC), Lux Cellulose-1 (NP), Lux Cellulose-2 (POSC) and Lux Cellulose-3 (RP), showed the broadest enantioselectivity and most complementarity. Six sequences of the three modes were considered to decide which sequence is the most successful for screening a set of 56 pharmaceutical compounds. Starting the strategy with the NP mode, followed by RP and finally POSC was found preferable from both the number of cumulative separations and of baseline separations. Two approaches were considered for strategy fine tuning using an additional set of eight racemic mixtures. In both approaches, seven of the eight compounds were baseline resolved, on one of the examined columns at either screening or optimization conditions of a mode. One approach was finally preferred because of its lower workload.
使用九种基于多糖的手性固定相 (CSP) 来定义一种分离策略，该策略结合了正相 (NP)、反相 (RP) 和极性有机溶剂色谱 (POSC) 模式。在每种模式中仅限制使用两种 CSP 后，总共使用了五种 CSP，Chiralpak AD（NP）、Chiralcel OD（RP 和 POSC）、Lux Cellulose-1（NP）、Lux Cellulose-2（POSC）和 Lux Cellulose-3（RP），显示出最广泛的对映选择性和互补性。考虑了三种模式的六个序列，以决定哪种序列最适合筛选一组 56 种药物化合物。从 NP 模式开始，然后是 RP，最后是 POSC，从累积分离数和基线分离数来看，这种方法都是首选。使用另一组八种外消旋混合物，考虑了两种方法来微调策略。在这两种方法中，在筛选或优化模式条件下，在所检查的柱子之一上，八种化合物中的七种都得到了基线分离。最终，由于其工作量较低，选择了一种方法。
