【作者】 李云志；

【导师】 曾凡骏；

【作者基本信息】 四川大学 ， 食品科学， 2005， 硕士

【摘要】 元宝枫是一种重要的经济植物,据研究其叶中含有丰富的生物活性物质黄酮类化合物,但到目前为止对该种资源提取方面的研究报道还不多,纯化工艺和化学成分研究更是未见报道。为开发利用该资源,论文对其提取分离纯化及化学成分结构鉴定进行了研究。用乙醇作为溶剂,采用常规浸提法及超声辅助法两种方法对元宝枫叶总黄酮的提取进行了对比研究。通过单因素及正交实验结果得到浸提法的优化条件为:溶剂使用50%(v/v)乙醇,料液比1:25(w/v),提取时间1.5h,浸提温度70℃。按照此条件提取两次,第一次提取率94.16%,第二次1.36%;超声辅助法的优化条件为:溶剂使用50%(v/v)乙醇,料液比1:15 (w/v),提取时间0.5h,浸提温度60℃。按照此条件提取两次,第一次提取率96.29%,第二次3.11%,两次即把黄酮基本提取完全。两种方法相比较,第一次提取率差别不大,但超声辅助法提取时间缩短1h,同时料液减少40%,提取温度低于浸提法10℃。选择8 种极性不同,孔径、比表面各异的大孔吸附树脂,比较其对元宝枫黄酮的吸附量和解吸率等指标,筛选较优的一种并对其相关条件下的动态吸附及解吸性能进行研究,以得率及纯度为指标进行考察。结果表明:DM-130 树脂对元宝枫黄酮有较好的吸附和解吸性能。最佳工艺参数:上样浓度1.2 ~2.3mg/mL,pH 4~5;上样速率1 ~2BV/h,流速越低,载量越大;解吸剂用体积分数70%乙醇, 流速1BV/h,可在3BV 内基本解吸黄酮,最更多还原

【Abstract】 Acer truncatum leaves are rich in many biologically active compounds and good sources of flavonoids. Extraction, purification, separation and identification of flavonoids in Acer truncatum leaves were studied in this thesis for better developing this resource. Two methods were applied to extract flavonoids from the leaves of Acer truncatum, that is, ethanol extraction without ultrasonic wave and ethanol extraction with ultrasonic wave. By orthogonal experiment, their optimum conditions were found. The optimum condition of ethanol extraction without ultrasonic wave is that the raw material was soaked in 50% (v/v) ethanol-water solution 25 times as many as its weight for 1.5 h at 70℃. Under this condition, the raw material was extracted two times. The extraction rate was 94.16% in the first time while it was 1.36% in the second time. The optimum condition of ethanol extraction with ultrasonic wave was that the raw material was soaked in 50% (v/v) ethanol–water solution 15 times as many as its weight for 0.5h at 60℃. Under this condition, the raw material was also extracted two times. In the first time, the extraction rate was 96.26% while it was 3.11% in the second time. Compared to extraction without ultrasonic wave, with ultrasonic wave showed much higher efficiency. The static adsorptive and desorptive capacities of 8 types of macroporous resins with different physical properties for flavonoids in the extract were determined to find a suitable resin for their purification. Then, the dynamic adsorption and desorption of the choosed resin to the flavonoids were studied. The results showed that resin DM130 had good adsorptive and desorptive capacities for the flavonoids. The optimum purification condition was that the slight acidified extract solution (pH4-5) containing 1.2-2.3mg/mL flavonoids poured on the resin at 1-2BV/h was eluted with 70%(v/v) ethanol at a flow rate of 1BV/h. The flavonoids adsorbed on the resin could be completely eluted within 3BV. The purified product contained 46.55% flavonoids. Two column chromatographies were used to separate flavonoids in the purified product and one flavonoid was isolated. It was identified as quercetin 3,5,7,3’,4’(OH)5-flavone by analysises of melting point, characteristic qualitative reactions and spectrographic data from UV, 1H-NMR, 13C-NMR, IR, ESI-MS. Extraction of flavonoids from the leaves of Acer truncatum without ultrasonic wave and with ultrasonic wave was compared in this thesis, and their own optimum conditions were obtained. A suitable macroporous resin DM130 was selected to purify flavonoids in the extract, and an appropriate purification condition was established. In addition, methods to separate the flavonoids were investigated and a pure flavonoid was gotten. Up to date, systemic studies and development on flavonoids in the leaves of Acer truncatum are little. So, the results from this study can provide for the future relate research. They also have definite theoretical and practical significance in pharmaceutical and now food resource development.更多还原