天然产物研究与开发 ›› 2019, Vol. 31 ›› Issue (增刊1): 97-101.doi: 10.16333/j.1001-6880.2019.S.017

• 开发研究 • 上一篇    下一篇

桑叶DNJ和Fagomine的检测及提取纯化工艺研究

徐月灿*,周衡,李丹,张莲莲,张倩,张峻康   

  1. 湖南希尔天然药业有限公司,永州 425000
  • 出版日期:2019-08-06 发布日期:2019-08-06

Study on detection,extraction and purification of DNJ and fagomine in mulberry leaves

XU Yue-can*,ZHOU Heng,LI Dan,ZHANG Lian-lian,ZHANG Qian,ZHANG Jun-kang   

  1. Hill Pharmaceutical Co.,Ltd.,Yongzhou 425000,China
  • Online:2019-08-06 Published:2019-08-06

摘要: 建立了高效液相色谱-衍生化法同时对桑叶中1-脱氧野尻霉素(1-deoxynojirimycin,DNJ)和Fagomine进行含量检测,并采用树脂法对桑叶中DNJ和Fagomine在同一条件下的提取纯化工艺进行研究。考察不同提取溶剂、不同型号树脂、树脂动态吸附特性、洗脱剂浓度等参数,并采用高效液相色谱-衍生化法对桑叶中DNJ和Fagomine进行检测,获得桑叶DNJ和Fagomine提取纯化工艺的优化条件:桑叶粗粉中加入6倍量0.1%盐酸水溶液加热回流提取三次,提取液浓缩后上LSD001树脂柱,再以0.5 mol/L的氨水洗脱并收集洗脱液。在此工艺条件下,所得样品中DNJ含量达5.65%,Fagomine含量达1.35%。

关键词: 高效液相色谱-衍生化, 桑叶, DNJ, Fagomine, 提取, 纯化

Abstract: A high performance liquid chromatography-derivatization method was established to simultaneously detect the contents of 1-deoxynojirimycin (DNJ) and Fagomine in mulberry leaves,and the extraction and purification processes of DNJ and Fagomine in mulberry leaves under the same conditions were studied by resin method.Different extraction solvents,different types of resin,resin dynamic adsorption characteristics,parameters such as concentration of eluant,and the high performance liquid chromatography (HPLC) of DNJ in mulberry leaves and Fagomine derivatization method for testing,mulberry DNJ and Fagomine optimization conditions of extraction and purification process,mulberry leaf meal to add 6 times the amount of 0.1% hydrochloric acid aqueous solution,heating reflux extraction,three times after the extract concentration on LSD001 resin column,then in 0.5 mol/L of ammonia elution and collect the eluent.The content of DNJ and Fagomine reached 5.65% and 1.35% respectively.

Key words: high performance liquid chromatography-derivatization method, mulberry leaves, DNJ, Fagomine, extraction, purification

中图分类号: 

R932