闪式提取-大孔树脂吸附分离山银花中绿原酸的工艺研究

摘要

目的:探索闪式提取-大孔树脂吸附分离山银花中绿原酸的最优工艺参数.方法:以绿原酸的转移率为评价指标,采用响应面试验设计,对闪式提取山银花中绿原酸的主要工艺参数进行优化.以绿原酸转移率及产品纯度为评价指标,以山银花药材水提液为上样液,采用单因素试验设计,对大孔树脂吸附分离绿原酸工艺中的主要工艺参数进行优化.结果: 闪式提取-大孔树脂吸附分离山银花中绿原酸的最优工艺条件为:料液比为1: 23,提取时间为4. 7 min,转数为6 000 r·min-1,大孔树脂类型为ADS-7,生药量与大孔树脂重量之比为1: 5,上样液流速为1 BV·h-1,先用1 BV的水以1 BV·h-1的流速洗脱,再用6 BV的20%乙醇以2 BV·h-1的流速洗脱,收集20%乙醇洗脱液.该工艺绿原酸的平均转移率为90. 12% (RSD=1. 33% ),绿原酸产品纯度为50. 30% (RSD=2. 19% ).结论: 创立了一条闪式提取-大孔树脂吸附分离山银花中绿原酸工艺路线,该工艺绿原酸转移率高,时间相对较短,溶剂无毒易于回收.%Objective: To explore the optimal extraction process by a blitzkrieg extractor and the adsorption separation by macro-porous resin for chlorogenic acid in Lonicera macranthoides. Methods: The transfer rate of chlorogenic acid was used as the main as-sessment index, the response surface test was adopted to optimize the main influencing factors in the extraction process by a blitzkrieg extractor for chlorogenic acid in Lonicera macranthoides. The transfer rate and the product purity of chlorogenic acid were used as the main assessment indices, the water extract solution of Lonicera macranthoides was used as the raw material, single factor test was adopt-ed to optimize the main influencing factors in the adsorption separation process by a macroporous resin for chlorogenic acid in Lonicera macranthoides. Results: The optimum conditions of the extraction process by a blitzkrieg extractor and the adsorption separation by a macroporous resin for chlorogenic acid in Lonicera macranthoides were as follows: the solid-liquid ratio was 1 : 23, the extraction time was 4. 7 min, the rotating speed was 6 000 r·min-1, the type of macroporous resin was ADS-7, the amount ratio of medicinal materi-als to macroporous resin was 1: 5, the flow rate of sample solution was 1 BV·h-1, the macroporous resin column was eluted by 1 BV water at the speed of 1 BV·h-1followed by 6 BV 20% ethanol solution at the speed of 2 BV·h-1, and the eluent of 20% ethanol so-lution was collected. The average transfer rate of chlorogenic acid was 90. 12% (RSD=1. 33% ) with the purity of 50. 30% (RSD=2. 19% ). Conclusion: A new route of the extraction process by a blitzkrieg extractor and the adsorption separation by a macroporous resin for chlorogenic acid in Lonicera macranthoides has established through the optimization and verification experiments. The process with high transfer rate of chlorogenic acid (the purity of chlorogenic acid product was over 50% ) is fast, and the solvent is healthy and easy to recycle.