应用化学 ›› 2011, Vol. 28 ›› Issue (04): 486-488.DOI: 10.3724/SP.J.1095.2011.00377

• 研究简报 • 上一篇    

毛细管电泳测定4个不对称合成化合物的光学纯度

吴同*,谭超,王金月   

  1. (宜宾学院化学与化工学院 宜宾 644000)
  • 收稿日期:2010-06-28 修回日期:2010-10-19 出版日期:2011-04-10 发布日期:2011-04-10
  • 通讯作者: 吴同,副教授; Tel:0831-3547500; Fax:0831-3530372; E-mail:wutmail@163.com; 研究方向:色谱技术
  • 基金资助:
    四川省青年科学基金(09ZQ026-066),宜宾学院基金(2010B13)资助项目

Capillary Electrophoresis Determination of the Enantiomeric Purity of Four Compounds Obtained from Asymmetry Synthesis

WU Tong*, TAN Chao, WANG Jinyue   

  1. (School of Chemistry and Chemical Engineering,Yibin University,Yibin 644000)
  • Received:2010-06-28 Revised:2010-10-19 Published:2011-04-10 Online:2011-04-10

摘要:

采用毛细管电泳技术,以α-环糊精、β-环糊精和β-环糊精聚合物为手性选择剂,对4种不对称合成物3-(二乙基氨基)-1-苯基-1-丙醇(a)、1-苯基-3-(1-哌啶)-1-丙醇(b)、3-吗啉-1-对甲苯基-1-丙醇(c)和1-(4-氯苯基)-3-吗啉-1-丙醇(d)的消旋体和光学活性异构体进行了手性分离。 结果发现,使用20 kV的分离电压,以浓度为30 g/L的β-环糊精聚合物的80 mmol/L三羟甲基氨基甲烷缓冲溶液(pH=3.2)为背景电解质溶液,4种化合物在40 min内均可得到基线分离。 根据对映异构体峰面积和保留时间的比值确定了4种不对称化合物的光学纯度。 测定的RSD均不大于1.5%。

关键词: 毛细管电泳, 光学纯度, β-环糊精聚合物, 手性分离

Abstract:

The enantioseparation of four compounds, 3-(diethylamino)-1-phenylpropan-1-ol(a), 1-phenyl-3-(piperidin-1-yl)propan-1-ol(b), 3-morpholino-1-p-tolypropan-1-ol(c) and 1-(4-chlorophenyl)-3-morpholinopropan-1-ol(d), obtained from asymmetry synthesis, was studied by capillary electrophoresis using α-cyclodextrin, β-cyclodextrin and β-cyclodextrin polymer as chiral selectors. With 20 kV as the separation voltage, and 30 g/L β-cyclodextrin polymer in 80 mmol/L Tris(pH=3.2) as background electrolyte solution, four chiral compounds were enantioseparated in 40 min. The enantiomeric purity of these four chiral compounds was determined according to the ratio of peak area with RSD no more than 1.5%.

Key words: capillary electrophoresis, enantiomeric purity, β-cyclodextrin polymer, enantioseparation

中图分类号: