色谱

色谱 ›› 2011, Vol. 29 ›› Issue (04): 365-367.DOI: 10.3724/SP.J.1123.2011.00365

• 技术与应用 • 上一篇    下一篇

高效液相色谱法分离双手性中心β-氨基酮旋光异构体

李蓬勃1, 田又平1, 陈立仁2, 徐峰1*   

  1. 1. 大分子科学陕西省重点实验室, 陕西师范大学化学与材料科学学院, 陕西 西安 710062; 2. 中国科学院兰州化学物理研究所, 甘肃 兰州 730000
  • 收稿日期:2010-12-21 修回日期:2011-02-28 出版日期:2011-04-28 发布日期:2011-04-28
  • 通讯作者: 徐峰,博士,教授,研究方向为不对称合成. Tel: (029)85307917, E-mail: fengxu@snnu.edu.cn.
  • 基金资助:
    国家自然科学基金项目(20872085)和陕西师范大学研究生培养创新基金项目(2010CXS004).

Resolution of optical isomers of β-amino ketone compounds with two chiral centres by high performance liquid chromatography

LI Pengbo1, TIAN Youping1, CHEN Liren2, XU Feng1*   

  1. 1. Key Laboratory of Macromolecular Science of Shaanxi Province, School of Chemistry & Materials Science, Shaanxi Normal University, Xi’an 710062, China; 2. Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China
  • Received:2010-12-21 Revised:2011-02-28 Online:2011-04-28 Published:2011-04-28

PDF

554

被引次数

5

摘要： 建立了使用AE. Lichrom AM 1手性色谱柱(250 mm×4.6 mm, 5 μm)直接拆分含有双手性中心的β-氨基酮类化合物的4个旋光异构体的方法。考察了流动相的极性大小、洗脱方式及流速等因素对异构体拆分的影响,确定了分离β-氨基酮类化合物异构体的最佳分离条件: 流动相为正己烷/异丙醇,洗脱模式为二元高压梯度洗脱,流速为1 mL/min。在上述色谱条件下,完成了4种含双手性中心的β-氨基酮类化合物的4个旋光异构体的基线分离(Rs＞1.5)。结果表明该方法可快捷、简便地分离双手性中心β-氨基酮类化合物的4个旋光异构体。

关键词: β-氨基酮类化合物, 拆分, 高效液相色谱, 旋光异构体

Abstract: A high performance liquid chromatographic method was developed for the resolution of optical isomers of β-amino ketone compounds containing two chiral centres. An AE. Lichrom AM 1 chiral chromatographic column (250 mm×4.6 mm, 5 μm) was used. The influences of the mobile phase polarity, flow rate and elution mode were investigated. The optimum conditions were the use of hexane-isopropyl alcohol as the mobile phase with a flow rate of 1 mL/min and gradient elution. Under the above chromatographic conditions, the optical isomers of four kinds β-amino ketone compounds containing two chiral centres were baseline separated (Rs＞1.5). It was proved that the method is fast and easy to separate the optical isomers of β-amino ketone compounds containing two chiral centres.

Key words: optical isomers, β-amino ketone compounds, high performance liquid chromatography (HPLC), resolution