高效率高纯度绿原酸制备工艺研究

Preparation of Highly Pure Chlorogenic Acid from Lonicera confusa

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。

This work aimed to establish an efficient method for the preparation of highly pure cMomgenlc acid from Lon/- cera 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 macmpomus resin, ethyl acetate liquid-liquid extraction, solvent crystallization were also optimized. Maximum extraction yield of 7.2% cldomgenic 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 macroperous resin,cluate of best purity was achieved by using 10% aqueous ethanol, and eluate of highest cldomgenic acid content was achieved by using 30% aqueous ethanol. It was optimized to perform liquld-liquid extraction for 5 times. Ethyl acetate saturated with water was the best solvent for crystallization. With the developed ex- traction and purification methods, clflomgenic acid at the purity of 98.7% with a yield of 1.84% was achieved. The pu- rity and yield were better than those recorded in other reported methods. Moreover,the extraction was performed at ambi- ent temperature in a short period of time and significantly reduced the energy consumption. Hence, it was suitable for large-scale industrial production.