应用化学 ›› 2010, Vol. 27 ›› Issue (08): 939-943.DOI: 10.3724/SP.J.1095.2010.90615

• 研究论文 • 上一篇    下一篇

二次球型配位包结结晶法选择分离中草药蒿本的肉豆蔻醚

鲁娜,郭放*,赵丹,佟健,郭文生   

  1. (辽宁大学化学学院 沈阳 110036)
  • 收稿日期:2009-09-10 修回日期:2010-01-11 出版日期:2010-08-10 发布日期:2010-08-10
  • 通讯作者: 郭放,女,研究员; E-mail:fguo@lnu.edu.cn; 研究方向:超分子化学及晶体工程
  • 基金资助:
    国家自然科学基金(20772054)资助项目

Selective Isolation of Component Myristicine from Ligustium sinense oliv by Second-Sphere Coordination Inclusion Crystallization

LU Na, GUO Fang*, ZHAO Dan, TONG Jian, GUO Wen-Sheng   

  1. (College of Chemistry,Liaoning University,Shenyang 110036)
  • Received:2009-09-10 Revised:2010-01-11 Published:2010-08-10 Online:2010-08-10

摘要:

采用[CoCl4]2-为第一配体,质子化的N,N,N′,N′-四(对甲基苄基)乙二胺为第二配体,构筑二次球形配位主体框架,选择性地将蒿本挥发油中的肉豆蔻醚作为客体,与其形成超分子包结物晶体。 采用红外光谱(IR)、核磁共振(NMR)、粉末X射线衍射(PXRD)等测试技术确定了包结物的形成及其主客体分子摩尔比为2∶1,利用Kugelrohr真空蒸馏技术将肉豆蔻醚从包结物晶体中分离出来。 用IR、NMR等方法确定了被分离的化学组分为肉豆蔻醚。 用GC方法测定了选择分离挥发油化学组分,蒿本挥发油中肉豆蔻醚的含量为60.4%,分离的肉豆蔻醚气相色谱纯度为100%。

关键词: 二次球形配位, 肉豆蔻醚, 蒿本挥发油, 分离, 包结结晶法

Abstract:

The first ligand of [CoCl4]2- and the second ligand of protonated N,N,N′, N′-tetra-p-methylbenzyl-ethylenediamine were used to construct a second-sphere coordination complex as the host framework. Myristicine was selectively isolated from the volatile oil of Ligustium sinense oliv by the inclusion crystalline method as the guest molecules. IR, NMR, X-ray diffraction were used to determine the structure of the inclusion complex, and the host-guest molar ratio in the complex was found to be 2∶1. The myristicine was isolated from the inclusion complex via Kugelrohr vacuum distillation technique and was characterized by IR, NMR and GC. According to the result of GC, the content of myristicine in the volatile oil of Ligustium sinense oliv is 60.4%, and the purity of isolated myristicine reaches 100%.

Key words: Second sphere coordination, myristicine, volatile oil of Ligustium sinense oliv, isolation, inclusion crystalline method

中图分类号: