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利用对映体迁移率相等但方向相反的特性,改进了特布他林对映体的制备规模连续自由流动电泳分离。

Improved preparative-scale. continuous, free-flow electrophoretic separation of the enantiomers of terbutaline utilizing equal-but-opposite enantiomer mobilities.

作者信息

Glukhovskij P, Vigh G

机构信息

Chemistry Department, Texas A&M University, College Station 77842-3012, USA.

出版信息

Electrophoresis. 2001 Aug;22(13):2639-45. doi: 10.1002/1522-2683(200108)22:13<2639::AID-ELPS2639>3.0.CO;2-T.

Abstract

The factors that influence yield and product purity in the continuous, preparative-scale electrophoretic separation of the enantiomers of terbutaline when using the principle of equal-but-opposite effective mobilities were studied. The sodium salt of heptakis-6-sulfato-beta-cyclodextrin was used as the resolving agent, in acidic, isopropanol-containing background electrolytes, in the continuous, free-flow, preparative electrophoretic instrument, the Octopus. By matching the linear velocity of the feed solution to that of the background electrolyte, lateral hydrodynamic dispersion was minimized resulting in a nonelectrophoresed feed band that was only three fractions (about 3 mm) wide as it exited the 0.5 m long separation channel. The multiple of residence time and applied potential was also optimized, constrained by migration of the front of heptakis-6-sulfato-beta-cyclodextrin out of the separation zone, leading to the recovery of 95% of both enantiomers in better than 99.99% purity, at a production rate of 0.1 mg/h.

摘要

研究了在使用等但相反有效迁移率原理对特布他林对映体进行连续制备规模电泳分离时,影响产率和产物纯度的因素。在连续的自由流动制备电泳仪器Octopus中,以含酸性异丙醇的背景电解质,使用七(6 - 硫酸根)-β-环糊精钠盐作为拆分剂。通过使进料溶液的线速度与背景电解质的线速度相匹配,横向流体动力学分散最小化,从而使得流出0.5米长分离通道时未电泳的进料带仅为三个馏分(约3毫米)宽。停留时间和施加电势的倍数也进行了优化,受七(6 - 硫酸根)-β-环糊精前沿移出分离区的限制,以0.1毫克/小时的生产率,两种对映体的回收率均达到95%,纯度优于99.99%。

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