Amini A, Paulsen-Sorman U
Medical Products Agency, Division of Chemistry and Pharmacy, Uppsala, Sweden.
Electrophoresis. 1997 Jun;18(6):1019-25. doi: 10.1002/elps.1150180626.
The enantiomers of prilocaine were successfully resolved with alpha-cyclodextrin, and those of mepivacaine and bupivacaine, with methyl-beta-cyclodextrin as chiral selectors, by means of capillary zone electrophoresis (CZE) employing a partial filling technique. By this separation mode, a discontinous separation zone is formed in the capillary. Prior to application of the actual drug substance, the capillary is partially filled with the separation solution. During the enantioseparation both ends of the capillary are dipped into the running buffer solution, i.e., without chiral selector. The consumption of chiral selector is thus very low, less than a microliter per run. The repeatibility of the electrophoretic mobility of the enantiomers was better than 1.2% relative standard deviation (RSD). The effect of the length of the separation zone on the resolution of the enantiomers was studied. The application time of the chiral selector, instead of the selector concentration, was varied in order to improve and regulate the enantioresolution and reduce consumption of the chiral selector as much as possible. It was found that the enantioseparations were directly affected by the length of the separation zone, and there was a minimal plug length where complete enantioresolution was achieved.
采用部分填充技术,通过毛细管区带电泳(CZE),成功地用α-环糊精拆分了丙胺卡因的对映体,并用甲基-β-环糊精作为手性选择剂拆分了甲哌卡因和布比卡因的对映体。通过这种分离模式,在毛细管中形成了一个不连续的分离区。在实际药物应用之前,毛细管部分填充有分离溶液。在手性拆分过程中,毛细管的两端浸入运行缓冲溶液中,即不含手性选择剂的溶液。因此,手性选择剂的消耗量非常低,每次运行不到一微升。对映体电泳迁移率的重复性相对标准偏差(RSD)优于1.2%。研究了分离区长度对对映体拆分的影响。为了提高和调节对映体拆分率并尽可能减少手性选择剂的消耗,可以改变手性选择剂的施加时间,而不是选择剂的浓度。结果发现,对映体拆分直接受分离区长度的影响,并且存在一个最小塞长度,在此长度下可实现完全对映体拆分。