杜仲籽粕中桃叶珊瑚甙的制备

用微波法进行杜仲籽粕中桃叶珊瑚甙的提取,通过溶剂萃取结合柱色谱分离纯化得到桃叶珊瑚甙纯品。确定适宜的微波提取条件为:φ(乙醇)=30%的水溶液为提取剂,微波功率560 W,按m(提取剂)/m(原料)=28提取1次,10 s,桃叶珊瑚甙的提取率达到95.55%;而超声波提取需90 min,提取率为90.69%;索氏回流法则需6 h,提取率仅为88.03%。粗提物用V(乙酸乙酯)∶V(提取液)=3∶1萃取2次,V(正丁醇)∶V(水相)=2∶1萃取3次后浓缩得浸膏;然后以V(甲醇)∶V(水)∶V(冰乙酸)=24.5∶75∶0.5为流动相,进行反相制备色谱分离,最后得到质量分数为92.32%的桃叶珊瑚甙产品,用核磁共振及质谱进行了确认。该研究工作的新颖性,已为教育部中南大学科技查新工作站2006年3月16日出具的第200643Z1100004号《科技查新报告》所证实。

Preparation of Aucubin from the Seed Draff of Eucommia Ulmoides Oliv

Microwave extraction technology of aucubin from the seed draff of Eucommiae ulmoides Oliv was investigated.Solvent extraction followed by column chromatographic purification was processed to obtain the aucubin monomer.The results showed that,the optimum technology of microwave extraction was φ(EtOH)=30% aqueous ethanol as extractant,m(extractant)/m(material)=28,microwave power 560 W and treating once for 10 s.The extraction rate of aucubin can reach 95.55%.By con trast,the extraction rates are 90.69% with ultrasonic extraction in 90 min and only 88.03% by Soxhlet extraction after 6 h.The raw extract solution was extracted twice with EtOAc(V(EtOAc)∶V(extract solution)=3∶1) and three times with n-BuOH(V(n-BuOH)∶V(water phase)=2∶1),and RP-HPLC system was used to process the extract gained above with the mobile phase of V(MeOH)∶V(H2O)∶V(HAc)=24.5∶75∶0.5.Aucubin was obtained with mass concentration of 92.32% and identified by NMR and MS.The novelty of this work was confirmed by the report(No.200643Z1100004) provided by the science and technology searching workstation of Central South University of Ministry of Education on Mar.16,2006.