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通过用2,3,4,6-四-O-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯衍生化,采用反相高效液相色谱法分离特布他林对映体。

Reversed-phase high performance liquid chromatographic separation of the enantiomers of terbutaline by derivatization with 2,3,4,6-tetra-o-acetyl-beta-D-glucopyranosyl isothiocyanate.

作者信息

Kim K H, Kim D S, Hong S P, Keon O S

机构信息

College of Pharmacy, Kangwon National University, Chunchon, Korea.

出版信息

Arch Pharm Res. 2000 Feb;23(1):26-30. doi: 10.1007/BF02976461.

Abstract

The enantiomers of the bronchodilator terbutaline were separated by reversed-phase high performance liquid chromatography after derivatization with 2,3,4,6-tetra-O-acetyl-beta-D-glucopyranosyl isothiocyanate(GITC) reagent. The derivatization proceeded quantitatively within 1 h at room temperature. The corresponding diastereomeric thiourea derivatives were well resolved on an ODS column with acetonitrile-acetate buffer as a mobile phase. Elution orders of the diastereomers were confirmed by derivatization of R-(-)-terbutaline and S-(+)-terbutaline which were collected by semi-preparative chiral HPLC using Sumichiral OA-4700 column. The native fluorescence of terbutaline was quenched by derivatization with GITC. The detection limit was 25 ng when monitored at UV 278 nm.

摘要

支气管扩张剂特布他林的对映体在用2,3,4,6-四-O-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯(GITC)试剂衍生化后,通过反相高效液相色谱法进行分离。衍生化在室温下1小时内定量进行。相应的非对映体硫脲衍生物在以乙腈-醋酸盐缓冲液为流动相的ODS柱上得到很好的分离。通过使用Sumichiral OA-4700柱的半制备手性HPLC收集的R-(-)-特布他林和S-(+)-特布他林的衍生化,确认了非对映体的洗脱顺序。特布他林的天然荧光通过与GITC衍生化而猝灭。在278nm紫外光下监测时,检测限为25ng。

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