过立农,张华,刘杰,马双成,昝珂,郑健.制备液相快速分离制备蒙药草乌叶的主要生物碱对照品[J].中国药事,2017,(10):1176-1180 |
制备液相快速分离制备蒙药草乌叶的主要生物碱对照品 |
Fast Isolation of Major Alkaloids as Reference Standards from Aconiti kusnezoffii Folium by Preparative HPLC |
投稿时间:2017-03-07 |
DOI:10.16153/j.1002-7777.2017.10.014 |
中文关键词: 草乌叶 阿朴啡生物碱 标准物质 去甲鹅掌楸啡碱 N-醛基去甲海罂粟碱 去甲海罂粟碱 结构鉴定 质量标准 |
英文关键词: Aconitum kusnezoffii folium aporphine alkaloids standard substance norlirioferine formylnorglaucine norglaucine structure elucidation quality standard |
基金项目:十二五国家科技重大专项(编号2014ZX09304307-002) |
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中文摘要: |
目的:提高蒙药草乌叶的质量标准,阐明药效物质,分离纯化质量研究用主要生物碱类对照品。方法:以HPLC为导向,采用硅胶柱、凝胶柱粗分后,采用制备液相进行生物碱的分离纯化;通过质谱(MS)、核磁共振(NMR)波谱学方法进行结构鉴定。结果:从草乌叶的乙醚提取物分离得到3个阿朴啡类生物碱,鉴定为去甲鹅掌楸啡碱(1)、N-醛基去甲海罂粟碱(2)、去甲海罂粟碱(3)。结论:化合物1~3为首次从乌头属植物中分离得到,具有较强的专属性,为该药材质量标准提高奠定了物质基础。同时,建立的制备液相快速分离方法,是制备质量研究用靶标对照品的有效手段。 |
英文摘要: |
Objective: In order to improve the quality standard and to elucidate effective substances of Mongolian medicine of Aconiti kusnezoffii folium, the major alkaloids as reference standards were isolated and purified. Methods: The alkaloids were isolated and purified by column chromatography with silica gel, Sephadex LH-20 and semi-preparative HPLC, guided by a developed HPLC method. The structure was identified by mass spectrometry (MS) and nuclear magnetic resonance (NMR) spectroscopy. Results: Three aporphine alkaloids were isolated from Ether extract of Aconiti kusnezoffii folium and their structures were elucidated as norlirioferine (1), (+)-N-formylnorglaucine (2), norglaucine (3) on the basis of spectral analysis. Conclusion: Compounds 1-3 were isolated from Aconitum for the first time, which had strong specificity, and could be used as quality control of this ethnic medicine. The results demonstrated that the preparative HPLC fast isolation was an effective tool to provide the target reference standards for quality control. |
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