CIESC Journal ›› 2016, Vol. 67 ›› Issue (S2): 191-196.DOI: 10.11949/j.issn.0438-1157.20161237

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Isolation and purification of alkaloid from Holarrhena antidysenterica Wall.ex A.DC

WANG Hongying1, ZHOU Yingnan1, UCHIDA Takafumi2, MARI Yotsu Yamashita2, QIAN Siriguleng1   

  1. 1. School of Biological Engineering, Dalian Polytechnic University, Dalian 116034, Liaoning, China;
    2. Graduate School of Agricultural Science, Tohoku University, Sendai 981-8555, Japan
  • Received:2016-09-05 Revised:2016-10-20 Online:2016-12-30 Published:2016-12-30
  • Supported by:

    supported by the Major Projects of Science and Technology in the Inner Mongolia Autonomous Region (222089).

蒙药材止泻木子生物碱的分离与纯化

王红英1, 周英男1, UCHIDA Takafumi2, MARI Yotsu Yamashita2, 钱斯日古楞1   

  1. 1. 大连工业大学生物工程学院, 辽宁 大连 116034;
    2. Tohoku University, Graduate School of Agricultural Science, Sendai 981-8555, Japan
  • 通讯作者: 钱斯日古楞
  • 基金资助:

    内蒙古自治区科技重大专项项目(222089)。

Abstract:

In this paper, one of the agent of alkaloid was extracted from the dry seeds of Holarrhena antidysenterica Wall.ex A.DC by ethanol, purified by silica gel chromatography and recrystallization.The structures of it was established on the basis of NMR techniques and mass spectrometry.The results showed that the optimum conditions of extraction were as follows:the Holarrhena antidysenterica Wall.ex A.DC was extracted under 60℃ for 6 h by 70% ethanol, and the getting rate of total alkaloid reached to 0.244%.By silica gel chromatography and recrystallization, the purity of one sample of compound 2 reached to 94.89%.The compound 2 was obtained as white crystal and its molecular formula C24H40N2was established by mass spectrometry (m/z 356.59[M+H]+).From the NMR data, the structure of compound 2 was deduced as conessine and its 13C NMR data were consistent with those of literature.

Key words: Holarrhena antidysenterica Wall.ex A.DC, NMR, silica gel columnchromatography, conessine, extraction, pharmaceuticals

摘要:

以夹竹桃科植物止泻木子的干燥种子为原材料,采用乙醇提取法对其生物碱类物质进行粗提取,通过硅胶柱层析和重结晶技术对生物碱粗提物进行分离和纯化。利用核磁共振波谱和质谱法对其一种生物碱单体进行化学结构和分子量鉴定。实验结果表明,用70%乙醇在60℃条件下静止浸取3次,每次提取6 h,得到止泻木子总生物碱提取物,其得率达到0.244%。经过硅胶柱分离和重结晶纯化,可获得3种生物碱单体。对HPLC检测纯度达到94.89%的2号生物碱单体进行核磁共振波谱和质谱检测,得知该生物碱单体是一个分子量为356.59的锥丝碱(conessine)。该结果有利于了解以止泻木子为主要成分的蒙药药剂作用机理。

关键词: 止泻木子, 核磁共振, 硅胶柱分离, 锥丝碱, 萃取, 药物

CLC Number: