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高效液相色谱法和毛细管电泳法拆分噻吩并[3,2-a]嘧啶类手性化合物,一种强效的 σ1 受体激动剂。

Separation of Tic-hydantoin enantiomers, potent sigma-1 agonists, by high performance liquid chromatography and capillary electrophoresis.

机构信息

UDSL, UFR Pharmacie,Laboratoire de Chimie Analytique, EA 4034, F-59000 Lille, France.

出版信息

J Chromatogr A. 2010 Jun 11;1217(24):3871-5. doi: 10.1016/j.chroma.2010.04.009. Epub 2010 Apr 24.

Abstract

Stereospecific separations of seven Tic-hydantoin sigma-1 agonists were performed by both HPLC method using derivatized cellulose and amylose chiral stationary phases and capillary electrophoresis (CE) method using neutral and anionic cyclodextrins added in the background electrolyte (BGE). An optimal baseline separation (R(s)>3.3 with analysis times<25min) was readily obtained with all silica-based celluloses and amyloses using a normal-phase methodology. CE was used as an alternative technique to HPLC for the Tic-hydantoin derivatives separation. The enantiomers were fully resolved with highly sulfated beta-cyclodextrins at pH 2.5 (R(s)>1.5 with analysis times <11min). Both methods were validated in terms of linearity, detection and quantification limits. They were used to check the enantiomeric purity of the enantiomers.

摘要

通过使用衍生纤维素和淀粉手性固定相的 HPLC 方法以及在背景电解质 (BGE) 中添加中性和阴离子环糊精的毛细管电泳 (CE) 方法,对七种 Tic-海因 sigma-1 激动剂进行了立体选择性分离。使用正相方法学,所有基于硅胶的纤维素和淀粉都很容易获得最佳的基线分离(Rs>3.3,分析时间<25min)。CE 被用作 HPLC 分离 Tic-海因衍生物的替代技术。在 pH 2.5 时,高度硫酸化的β-环糊精可完全分离对映异构体(Rs>1.5,分析时间<11min)。这两种方法都在线性、检测和定量限方面进行了验证。它们被用于检查对映异构体的对映体纯度。

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