双水相气浮溶剂浮选法分离富集杜仲叶中京尼平苷酸  

Separation and enrichment of geniposidic acid from leaves of Eucommia ulmoides by aqueous two-phase flotation

作　　者：赵帅[1] 刘磊磊[1] 郭婕[1] 彭密军[1] 

机构地区：[1]吉首大学林产化工工程湖南省重点实验室,湖南张家界427000

出　　处：《中草药》2015年第16期2400-2406,共7页Chinese Traditional and Herbal Drugs

基　　金：湖南省自然科学基金资助项目(14JJ6037);吉首大学2013年人才引进专项项目资助(jsdxrcyjkyxm201301);林产化工工程湖南省重点实验室开放基金(13jdzb075);吉首大学2014年度校级科研项目(14JDY060)

摘　　要：目的采用乙醇/Na H2PO4双水相气浮溶剂浮选技术,结合响应曲面法对杜仲叶中京尼平苷酸进行分离富集研究。方法考察了无机盐种类和用量、有机溶剂的种类和用量、粗提液加入量、空气体积流量和浮选时间对京尼平苷酸浮选效果的影响,在单因素试验基础上,选择Na H2PO4质量分数、乙醇体积分数和空气体积流量为实验因素,采用Box-Behnken中心组合设计进行优化实验,确定京尼平苷酸的最优浮选工艺,并进行100倍放大研究。结果在28%Na H2PO4、23%乙醇双水相体系中,加入5 g粗提液,当空气体积流量为40 m L/min,浮选时间为20 min时,京尼平苷酸浮选效率最佳,达到97.88%,富集倍数达到27.34。100倍放大后,京尼平苷酸的浮选效率达到95.60%,RSD为0.77%。结论乙醇/Na H2PO4双水相气浮溶剂浮选体系对京尼平苷酸的浮选效率高,富集倍数大,为杜仲叶中环烯醚萜类活性成分分离富集提供了一种有效的新方法。Objective Ethanol/Na H2PO4 aqueous two-phase gas solvent sublation coupled with response surface methodology was developed for the separation/enrichment and analysis of geniposidic acid from the leaves of Eucommia ulmoides. Methods For the aqueous two-phase flotation project, the flotation effects of different solvent, salts, flotation rate, flotation time, amount of crude extract and so on were deeply investigated; Furthermore, a Box-Behnken central composite test design was studied to determine the best flotation process conditions of GPA, and three factors including the mass fraction of Na H2PO4, the mass fraction of ethanol, and the flotation rate were selected based on the single factor test in the design. A 100 times scale-up experiment also was tested. Results The optimal conditions of the flotation were as follows： the mass fraction of Na H2PO4 was 25%, the mass fraction of ethanol was 20%, the amount of crude extract was 5 g, the flotation rate was 30 m L/min, and the flotation time was 20 min. Under the optimal condition, the flotation efficiency was 97.88%, and the enrichment factor was 27.34; The 100 times scale-up results showed that the flotation efficiency of GPA was 95.60%, and the RSD value was 0.77%. Conclusion The method with ethanol/Na H2PO4 aqueous two-phase gas solvent sublation is suitable for the separation and enrichment of the active ingredients from E. ulmoides because of its high distribution coefficient and large enrichment factor.

关 键 词：双水相气浮溶剂浮选 杜仲 京尼平苷酸 分离富集 响应曲面法 

分 类 号：R284.2[医药卫生—中药学]