色谱

色谱 ›› 2014, Vol. 32 ›› Issue (6): 612-615.DOI: 10.3724/SP.J.1123.2014.02023

• 研究论文 • 上一篇    下一篇

高效液相色谱手性流动相添加法拆分阿卓乳酸对映体

张虎, 沈芒芒, 童胜强, 颜继忠   

  1. 浙江工业大学药学院, 浙江 杭州 310032
  • 收稿日期:2014-02-24 修回日期:2014-03-17 出版日期:2014-06-08 发布日期:2014-05-22
  • 通讯作者: 童胜强
  • 基金资助:

    国家自然科学基金项目（21105090）；2013年浙江省高等学校中青年学科带头人学术攀登项目（Pd2013031）.

High performance liquid chromatographic enantioseparation of atrolactic acids using chiral mobile phase additive

ZHANG Hu, SHEN Mangmang, TONG Shengqiang, YAN Jizhong   

  1. College of Pharmaceutical Science, Zhejiang University of Technology, Hangzhou 310032, China
  • Received:2014-02-24 Revised:2014-03-17 Online:2014-06-08 Published:2014-05-22

PDF

239

被引次数

10

摘要：

采用C18反相色谱柱，以磺丁基醚-β-环糊精（SBE-β-CD）作为手性流动相添加剂，建立了阿卓乳酸对映体的高效液相色谱拆分方法。考察了环糊精衍生物类型、手性添加剂浓度、流动相pH、流速和柱温对手性分离的影响，同时探讨了高效液相色谱采用磺丁基醚-β-环糊精分离阿卓乳酸对映体的分离机制及包结常数，确定了色谱条件为YMC-Pack ODS-A C18色谱柱（250 mm×4.6 mm，5 μm），流动相为含25 mmol/LSBE-β-CD的0.1 mol/L磷酸盐缓冲液（pH 2.68）-乙腈（90：10，v/v），流速为0.6 mL/min，柱温为30 ℃，紫外检测波长为220 nm。对映体的保留时间分别为26.65和28.28 min，分离度为1.68。本方法分离度好，简便易行，且比使用手性固定相分离更加经济。

关键词: 阿卓乳酸, 对映体拆分, 高效液相色谱, 磺丁基醚-β-环糊精, 手性流动相添加法

Abstract:

A method was established for the enantioseparation of atrolactic acids using high performance liquid chromatography with sulfobutyl ether-β-cyclodextrin (SBE-β-CD) as the chiral mobile phase additive, and a C18 reversed-phase column. The influences of the different types of cyclodextrin derivatives, the concentration of chiral mobile phase additive, pH value of the mobile phase, the flow rate and column temperature on the peak resolution were investigated. The separation mechanism for atrolactic acids by high performance liquid chromatography using chiral mobile phase additive, as well as the formation of inclusion complex between SBE-β-CD and atrolactic acid was studied. In addition, the formation constant was calculated. The enantioseparation was carried out on a reversed-phase column YMC-Pack ODS-A C18 (250 mm×4.6 mm, 5 μm) with chiral mobile phase consisted of 0.1 mol/L phosphate buffer at pH 2.68 containing 25 mmol/L SBE-β-CD-acetonitrile (90:10, v/v). The detection wavelength was 220 nm. The flow rate was 0.6 mL/min and the column temperature was 30 ℃. The retention times of atrolactic acids were 26.65 and 28.28 min, and the peak resolution of 1.68 was achieved. The above established method proves to be a simple and economical way for analytical enantioseparation of atrolactic acid with high peak resolution.

Key words: atrolactic acid, chiral mobile phase addition, enantioseparation, high performance liquid chromatography (HPLC), sulfobutyl ether-β-cyclodextrin (SBE-β-CD)

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