色谱

色谱 ›› 2012, Vol. 30 ›› Issue (03): 280-284.DOI: 10.3724/SP.J.1123.2011.10020

• 研究论文 • 上一篇    下一篇

以L-酒石酸正己酯-硼酸配合物作为反相液相色谱手性流动相添加剂拆分5种β-受体阻滞剂

杨娟, 王利娟, 郭巧玲, 杨更亮*   

  1. 河北大学药学院, 河北省药物质量研究重点实验室, 河北 保定 071002
  • 收稿日期:2011-10-20 修回日期:2011-11-13 出版日期:2012-03-28 发布日期:2012-05-02
  • 通讯作者: 杨更亮,教授,博士生导师. Tel: (0312)5971108, E-mail: ygl@hbu.edu.cn.
  • 基金资助:

    国家自然科学基金项目(No. 21175031)、河北省应用基础研究计划重点基础研究项目(No. 11966411D)、河北省高等学校科学技术研究重点项目(No. ZD2010234)和河北省药物质量研究重点实验室青年开放课题(No. 09265631D-13).

Chiral separation of five β-blockers using di-n-hexyl L-tartrate-boric acid complex as mobile phase additive by reversed-phase liquid chromatography

YANG Juan, WANG Lijuan, GUO Qiaoling, YANG Gengliang*   

  1. College of Pharmacy, Hebei University, Hebei Province Key Laboratory of Pharmaceutical Quality Control, Baoding 071002, China
  • Received:2011-10-20 Revised:2011-11-13 Online:2012-03-28 Published:2012-05-02

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摘要：

本文以L-酒石酸正己酯-硼酸配合物为手性流动相添加剂，建立了普萘洛尔、艾司洛尔、美托洛尔、比索洛尔、索他洛尔和阿替洛尔六种β-受体阻滞剂的反相高效液相色谱手性分离方法。对影响对映体分离的主要因素：L-酒石酸正己酯、硼酸浓度，缓冲溶液种类、浓度、pH值和有机改性剂-甲醇含量等进行了详细考察。最佳色谱条件为：Venusil MP-C18色谱柱（4.6 mm × 250 mm，5 μm），流动相为15 mmol/L乙酸铵-甲醇（体积比为20: 80或30: 70，含60 mmol/L硼酸，70 mmol/L L-酒石酸正己酯，醋酸调节pH值6.00），检测波长214 nm。在最佳分离条件下，五对对映体（普萘洛尔、艾司洛尔、美托洛尔、比索洛尔、索他洛尔）可以分别获得基线分离。

关键词: β-受体阻滞剂, 反相高效液相色谱, 酒石酸酯-硼酸配合物, 手性拆分, 手性添加剂

Abstract:

A reversed-phase high performance liquid chromatographic (HPLC) method using the di-n-hexyl L-tartrate-boric acid complex as a chiral mobile phase additive was developed for the enantioseparation of five β-blockers including propranolol, esmolol, metoprolol, bisoprolol and sotalol. In order to obtain a better enantioseparation, the influences of concentrations of di-n-butyl L-tartrate and boric acid, the type, concentration and pH of the buffer, methanol content as well as the molecular structure of analytes were extensively investigated. The separation of the analytes was performed on a Venusil MP-C18 column (250 mm×4.6 mm, 5 μm). The mobile phase was 15 mmol/L ammonium acetate-methanol containing 60 mmol/L boric acid, 70 mmol/L di-n-hexyl L-tartrate (pH 6.00). The volume ratios of 15 mmol/L ammonium acetate to methanol were 20:80 for propranolol, esmolol, metoprolol, bisoprolol and 30:70 for sotalol. The flow rate was 0.5 mL/min and the detection wavelength was set at 214 nm. Under the optimized conditions, baseline enantioseparation was obtained separately for the five pairs of analytes.

Key words: β-blockers, chiral additive, chiral separation, tartrate-boric acid complex, reversed-phase high performance liquid chromatography (RP-HPLC)