天然产物研究与开发 ›› 2016, Vol. 28 ›› Issue (12): 1943-1946.doi: 10.16333/j.1001-6880.2016.12.016

• 研究简报 • 上一篇    下一篇

pH区带精制逆流色谱法分离制备黄藤中巴马汀和药根碱

井凤，耿岩玲，刘伟，段文娟，王岱杰，王晓*   

  1. 山东省中药质量控制技术重点实验室 山东省分析测试中心，济南 250014
  • 出版日期:2016-12-31 发布日期:2017-03-31

Separation and Preparation of Palmatine and Jateorhizine in Fibraurea recisa Pierre.by pH-Zone-Refining Counter-Current Chromatography

JING Feng,GENG Yan-ling,LIU Wei,DUAN Wen-juan,WANG Dai-jie,WANG Xiao*   

  1. Key Laboratory of TCM Quality Control Technology,Shandong Analysis and Test Center,Jinan 250014,China
  • Online:2016-12-31 Published:2017-03-31

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摘要： 建立了黄藤生物碱快速分离制备的pH区带精制逆流色谱方法。采用95%乙醇加热回流提取制备黄藤生物碱粗提物，利用pH区带精制逆流色谱法对生物碱粗提物进行直接分离制备，以氯仿-甲醇-水（4:3:3）为溶剂系统，下相添加三乙胺（10 mmol/L）为流动相，上相加盐酸（40 mmol/L）作为固定相，在主机转速800 rpm，流动相流速2 mL/min，检测波长254 nm条件下进行分离制备。从1.5 g黄藤提取物中一次分离得到231.6 mg药根碱和436.8 mg巴马汀，纯度均大于98%。化合物通过MS、1H NMR和13C NMR进行了结构鉴定。pH区带精制逆流色谱法是一种快速高效的分离纯化黄藤生物碱的方法。

关键词: 黄藤, pH区带精制逆流色谱, 生物碱, 药根碱, 巴马汀

Abstract: A rapid method was developed for the preparative separation of alkaloids from Fibraurea recisa Pierre.by pH-zone-refining counter-current chromatography.The crude sample was prepared by 95% ethanol reflux extraction and directly separated by pH-zone-refining counter-current chromatography.The solvent system was chloroform-methanol-water (4:3:3,v/v) with 40 mM HCl in the upper stationary phase and 10 mM TEA in the lower mobile phase.The rotation speed was set at 800 rpm.The flow rate was 2.0 mL/min and the detective wavelength was 254 nm.From 1.5 g of the crude sample,231.6 mg of jatrorrhizine and 436.8 mg of palmatine were obtained and each with a purity higher that 98% as determined by HPLC.The chemical structures were identified according to MS, 1H NMR and 13C NMR.The pH-zone-refining counter-current chromatography was a rapid and efficient method for the separation of alkaloids from Fibraurea recisa Pierre.

Key words: Fibraurea recisa Pierre., pH-Zone-refining counter-current chromatography, alkaloids, palmatine, jatrorrhizine

中图分类号: 

R284.2

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