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采用纤维素苯基型手性固定相和圆二色检测法对苯并恶硫平衍生物的四种立体异构体进行高效液相色谱定量分析。

HPLC quantitation of the four stereoisomers of benzoxathiepin derivatives with cellulose phenyl type chiral stationary phase and circular dichroism detection.

作者信息

Beaufour Martine, Morin Philippe, Ribet Jean-Paul, Maurizot Jean-Claude

机构信息

Institut de Chimie Organique et Analytique (ICOA), CNRS FR 2708, UMR 6005, Université d'Orléans, BP 6759, 45067 Orléans cedex 2, France.

出版信息

J Pharm Biomed Anal. 2006 May 3;41(2):544-8. doi: 10.1016/j.jpba.2005.11.034. Epub 2006 Jan 19.

DOI:10.1016/j.jpba.2005.11.034
PMID:16427239
Abstract

The chiral separation of a new antianginal agent has been investigated on a chiral cellulose column with UV and circular dichroism (CD) detection. This benzoxathiepin derivative under development has two stereogenic centers whose (R,S) stereoisomer shows an interesting antianginal activity. After optimisation of the mobile phase composition, a baseline-resolved separation of the four stereoisomers was achieved on a Chiralcel OJ-H chiral column by using methanol-ethanol-diethylamine (25:75:0.1, v/v/v) as mobile phase. The CD detection system allowed quantitation and a linear response was observed within a 10-200 microg mL-1 concentration range (r2=0.9966) and limit of quantification down to 2 microg mL-1 was achieved.

摘要

在配备紫外和圆二色性(CD)检测的手性纤维素柱上,对一种新型抗心绞痛药物进行了手性拆分研究。这种正在研发的苯并[1,3]噻嗪衍生物有两个手性中心,其(R,S)立体异构体表现出有趣的抗心绞痛活性。在优化流动相组成后,以甲醇 - 乙醇 - 二乙胺(25:75:0.1,v/v/v)为流动相,在Chiralcel OJ - H手性柱上实现了四种立体异构体的基线分离。CD检测系统实现了定量分析,在10 - 200 μg mL-1浓度范围内观察到线性响应(r2 = 0.9966),定量限低至2 μg mL-1。

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