天然产物研究与开发 ›› 2014, Vol. 26 ›› Issue (9): 1503-1509.

• 开发研究 • 上一篇    下一篇

高效率高纯度绿原酸制备工艺研究

陈 媛*,唐铁鑫,陈金龙,蒋 林*   

  1. 中山大学药学院生药与天然药物化学实验室,广州 510006
  • 出版日期:2014-09-30 发布日期:2014-11-02

Preparation of Highly Pure Chlorogenic Acid from Lonicera confusa

CHEN Yuan*, TANG Tie-xin, CHEN Jin-long, JIANG Lin*   

  1. School of Pharmaceutical Sciences,Sun Yatsen University,Guangzhou 510006, China
  • Online:2014-09-30 Published:2014-11-02

摘要: 建立从山银花中制备绿原酸标准品的方法,并提高绿原酸产率。通过正交试验优化传统水提法和碱水冷提法工艺,并对D101大孔树脂纯化条件、乙酸乙酯萃取次数、结晶溶剂进行优化。通过研究,最佳提取条件为:提取溶剂pH=10的碱水,提取时间1 h,料液比1:30,提取率为7.2%;D101大孔树脂洗脱溶剂:10%乙醇洗脱液纯度最高,30%乙醇洗脱液得率最高;最佳萃取次数5次;最佳结晶溶剂:水饱和乙酸乙酯。本研究通过创新的提取和纯化条件,得到纯度98.7%的绿原酸,得率18.4 mg/g,纯度和得率都高于现有文献记载,且常温快速提取,能耗明显下降,适用于工业规模高纯度绿原酸生产。

关键词: 绿原酸, 山银花, 碱水, D101大孔树脂, 结晶

Abstract: This work aimed to establish an efficient method for the preparation of highly pure chlorogenic acid from Lonicera confusa. Two extraction methods,conventional water extraction and alkaline water extraction at ambient temperature,were optimized by orthogonal experimental design.The purification processes using D101 macroporous resin,ethyl acetate liquid-liquid extraction,solvent crystallization were also optimized.Maximum extraction yield of 7.2% chlorogenic acid was achieved by using alkaline water at pH=10 as solvent,extraction time of 1 h,and solid-to-liquid ratio of 1:30.As to the eluent of D101 macroporous resin,eluate of best purity was achieved by using 10% aqueous ethanol,and eluate of highest chlorogenic acid content was achieved by using 30% aqueous ethanol.It was optimized to perform liquidliquid extraction for 5 times.Ethyl acetate saturated with water was the best solvent for crystallization.With the developed extraction and purification methods,chlorogenic acid at the purity of 98.7% with a yield of 1.84% was achieved.The purity and yield were better than those recorded in other reported methods.Moreover,the extraction was performed at ambient temperature in a short period of time and significantly reduced the energy consumption.Hence,it was suitable for large'scale industrial production.

Key words: chlorogenic acid, Lonicera confusa, alkaline water extraction, D101 macroporous resin, crystallization

中图分类号: 

R284.2