盾叶薯蓣皂苷元制备新工艺研究.pdfVIP

摘 要 盾叶薯蓣因其皂苷元含量高，成为我国工业化生产薯蓣皂苷元的重要原料。皂苷元是 合成多种甾体激素和甾体避孕药理想的前体。目前工业上多采用自然发酵酸水解法，排放 大量酸水，造成严重污染。本文建立了盾叶薯蓣皂苷元制备新工艺，既保证了得率，又实 现了酸水 “低排放”。 本论文研究工作如下： 1. 开发了干燥盾叶薯蓣“醇提过柱”制备薯蓣皂苷元的新工艺：利用95% 乙醇代替水浸 提薯蓣皂苷及薯蓣皂苷元，利用大孔树脂柱分离排除乙醇提取液中淀粉、纤维素等物质， 在乙醇-盐酸环境中对薯蓣皂苷进行酸解，中和后萃取重结晶得到皂苷元。其皂苷元得率为 2.76% ，比工业酸水解法的0.7 1%高出3.88 倍，同时大大降低盐酸用量，实现了酸水“低排 放” 。 2. 研究了新鲜盾叶薯蓣 “醇提过柱”制备皂苷元工艺：其皂苷元得率为0.83% ，制备 单位重量皂苷元盐酸消耗量为44 .7 1 mL 。与干燥盾叶薯蓣相比较，新鲜料不仅得率低，盐 酸消耗量为干料的3.32 倍，而且存在季节性生产问题，干料具有性价比高的优点。 3. 研究了干燥盾叶薯蓣直接酸解制备皂苷元工艺：其皂苷元得率为2.13% ，制备单位 重量皂苷元盐酸消耗量量17.42 mL 。与新工艺较为接近，但是盾叶薯蓣中的淀粉、纤维素 等原材料未能实现再利用。 关键词：盾叶薯蓣；薯蓣皂苷元；大孔树脂；“醇提过柱” ；酸水“低排放” 。 I ABSTRACT Dioscorea zingiberensis contains relatively high concentration of Diosgenin and has become very important raw material for the industrialized producti n of Diosgenin. Diosgenin is the ideal precursor for the synthesis of several steroid hormones and contraceptive steroids. The technique currently adopted is natural fermentation and acidolysis with di harge of large amount of acid water which causes serious environmental pollution. In this thesis a new technique was established to prepare Diosgenin without the discharge of acid water and at the sam e time high yield could be achieved. The research work is as follows: In part one, new technique was established to prepare Diosgenin from dry Dioscorea zingiberensis after ethanol extraction and purification by the colum . Water was replaced by 95% ethanol. Large amount of starch, cellulose and protein etc. in ethanol extract were separated by the macroporous resin column. All saponins were acidolyzed in ethanol and hydrochloric acid (HCl). Subsequently Diosgenin was obtained after neutralization