柱前手性衍生化反相高效液相色谱法测定转运液中7种芳氧丙醇胺类β受体阻断剂对映体的含量

柱前手性衍生化反相高效液相色谱法测定转运液中7种芳氧丙醇胺类β受体阻断剂对映体的含量

贺瑛, 柴晓鹃, 曾苏^*

浙江大学药学院药物分析与药物代谢研究室, 浙江杭州 310058

收稿日期:2009-10-11 修回日期:2010-02-20 出版日期:2010-03-15 发布日期:2010-03-15
通讯作者: 曾苏*

Reversed-phase high-performance liquid chromatographic analysis of seven pairs of chiral drug enantiomers in transport medium after chiral derivatization

Ying He, Xiao-Juan Chai, Su Zeng^*

Department of Pharmaceutical Analysis and Drug Metabolism, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China

Received:2009-10-11 Revised:2010-02-20 Online:2010-03-15 Published:2010-03-15
Contact: Su Zeng*

摘要/Abstract

摘要：

建立转运液中7种芳氧丙醇胺类β受体阻断剂对映体 (阿替洛尔、索他洛尔、塞利洛尔、卡维地洛、美托洛尔、普萘洛尔、普罗帕酮) 的反相高效液相色谱测定法。转运液中药物经液液萃取后, 加入100 µL GITC乙腈液 (1.0 mg/mL) 进行手性衍生化, 再用C8柱进行分离, 流动相为乙腈-0.01 mol/L磷酸二氢钾缓冲盐 (pH 3.5)。本方法专属性较好, 对映体和内标的绝对回收率均>78%, 对映体的相对回收率约为100%, 日间和日内精密度均<15%。结果表明本方法简便、快速、重现性好, 可应用于这7种药物在Caco-2细胞单层转运中的立体选择性研究

关键词: 对映体分离, 芳氧丙醇胺类药物, RP-HPLC, 柱前衍生化

Abstract: A reversed-phase high-performance liquid chromatographic (RP-HPLC) method was established for the determination of the enantiomers of 7 aryloxy aminopropanol drugs (atenolol, sotalol, celiprolol, carvedilol, metoprolol, propranolol and propafenone) in transport medium. The method involved liquid-liquid extraction of chiral drugs from transport medium, and employed 2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl isothiocyanate (GITC, 1.0 mg/mLin acetonitrile) as a pre-column chiral derivatization reagent. After derivatization, the products were separated on an Agilent Zorbax C8 column (150 mm×4.6 mm, 5 µm) at 25 °C. The mobile phase consisted of a mixture of acetonitrile and 0.01 M phosphate buffer (pH 3.5). The present methods were specific for the determination of enantiomers of each chiral drug. The absolute recoveries of the enantiomers and internal standards were >78%. The relative recoveries of the enantiomers were approximately 100%. The intra- and inter-day variations were <15%. The method was reproducible and sufficiently sensitive to determine the enantiomers of seven aryloxy aminopropanol drugs in transport medium. The method could be used to study the transport of atenolol, sotalol, celiprolol, carvedilol, metoprolol, propranolol and propafenone.

Key words: Enantiomer separation, Aryloxy aminopropanol drugs, RP-HPLC, Pre-column derivatization

中图分类号:

R917

Supporting:

Foundation item: National Key Project of China (Grant No. 2009ZX09304-003).
^*Corresponding author. Tel.: 86-571-88208407

贺瑛, 柴晓鹃, 曾苏^*. 柱前手性衍生化反相高效液相色谱法测定转运液中7种芳氧丙醇胺类β受体阻断剂对映体的含量[J]. .

Ying He, Xiao-Juan Chai, Su Zeng^* . Reversed-phase high-performance liquid chromatographic analysis of seven pairs of chiral drug enantiomers in transport medium after chiral derivatization [J]. .

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