论文部分内容阅读
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 To study the separation and enrichment of geniposidic acid in Eucommia ulmoides leaves by ethanol / Na H2PO4 double aqueous flotation solvent flotation combined with response surface methodology. Methods The effects of the types and amount of inorganic salts, the type and amount of organic solvents, the amount of crude extract, the volume flow of air and the flotation time on the flotation of geniposidic acid were investigated. Based on the single factor experiments, Na H2PO4 mass fraction, ethanol volume fraction and air volume flow rate were used as experimental factors to optimize the experiment with Box-Behnken central composite design to determine the optimal flotation process of geniposidic acid and to conduct a 100-fold magnification study. Results In 28% Na H2PO4 and 23% ethanol aqueous two-phase system, 5 g crude extract was added. When the air volume flow rate was 40 m L / min and the flotation time was 20 min, the genipin flotation efficiency The best, reaching 97.88% enrichment multiples reached 27.34.100 times magnification, genipin acid flotation efficiency of 95.60%, RSD 0.77%. Conclusions The flotation system of ethanol / Na H2PO4 double aqueous flotation solvent has high flotation efficiency and enrichment factor for geniposidic acid, which provides an effective method for the separation and enrichment of iridoid active ingredients in Eucommia ulmoides leaves new method.