分相萃取法制备高纯度绿原酸的工艺研究.PDF

※工艺技术 食品科学 2010, Vol. 31, No. 14 37 胡居吾，李雄辉 * ，熊 伟，季清荣，涂招秀，李向阳 (江西省科学院应用化学研究所，江西 南昌 330029) ：以杜仲叶为原料提取绿原酸，将大孔树脂和混合溶剂分相法相结合，对绿原酸进行精制纯化，使绿原 酸的纯度达到 99.5%(HPLC 法) 。在萃取工艺中选定有机溶剂乙酸乙酯为萃取剂，考察萃取时间、pH 值、萃取次 数对萃取率的影响，并通过响应面法建立萃取率和萃取时间、pH 值、萃取次数之间的关系，得到最佳萃取工艺 条件为萃取时间 4.00min 、pH2.97 、萃取次数4 次，此时绿原酸萃取率达到 95.1% 。在分相工艺中，首先对分相 剂进行筛选，选定非极性溶剂正己烷为分相剂，再对分相剂的用量进行研究，最终确定其用量为萃取液总体积的 40% ，绿原酸转移率达 93% 以上。 绿原酸；萃取；分相法；响应面分析 Phase Separation and Extraction with n- Hexane for the Preparation of High Purity Chlorogenic Acid HU Ju-wu ，LI Xiong-hui* ，XIONG Wei ，JI Qing-rong ，TU Zhao-xiu ，LI Xiang-yang (Institute of Applied Chemistry, Jiangxi Academy of Sciences, Nanchang 330029, China) Abstract ：Macroporous resin 306 adsorption followed by phase separation and extraction was used to purify the crude chlorogenic acid extract from Eucommia ulmoides leaves. Ethyl acetate was selected for the phase separation of chlorogenic acid. The individual effects of length of extraction, pH and extraction times on the yield of chlorogenic acid were investigated in the single factor experiments. Box-Behnken experimental design was employed to provide a basis for the development of a mathematical model predicting the yield of chlorogenic acid as a function of length of extraction, pH and extraction times and subsequently, the interactive effects of the independent variables on their function were analyzed using response surface methodology (RSM). The optimal values of the independent variables were found to be: extraction time 3.40 min, pH 2.97, extraction times 4. Under these optimal conditions, the maximum yield of chlorogenic acid reached up to 95.1%. Non-polar n- hexane was found to be the best choice for the transfer of chlorogenic