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橘皮的化学成分与黄酮类化合物的提取、纯化研究

Study on Chemicals of Citrus Peels and Extraction and Purification of Flavonoids from Them as Well

【作者】 刘均玉

【导师】 陈清松; 许晨;

【作者基本信息】 福建师范大学 , 高分子化学与物理, 2009, 硕士

【摘要】 本文主要是关于柑橘皮中黄酮类化合物的含量分析、提取条件优化、分离制备单一天然产物的方法研究。实验结果表明:1、不同品种的橘皮中黄酮的种类、含量不同,并且相差很大,需要针对不同的目标产物选择原料。2、比较常压有机溶剂、高压有机溶剂、超临界二氧化碳和常压石灰水提取柑橘皮中黄酮类化合物的条件、提取物的纯度、提取效率,结果显示:常压超声提取最经济,高压有机溶剂提取效率最高,超临界二氧化碳的提取物纯度高但效率低,饱和石灰水是提取柑橘皮中橙皮苷的理想溶剂,甲醇、乙醇、正丁醇对黄酮类化合物的提取效率依次增大,提取物的纯度也提高,高压乙酸乙酯是提取多甲氧基黄酮的理想方法。3、比较不同极性有机溶剂萃取分离、高速逆流色谱分离、D101大孔树脂吸附、强碱性阴离子交换树脂吸附等方法对提取物的纯化效果。结果显示:不同极性的有机溶剂和高速逆流色谱并不能实现复杂混合物的完全分离;D101大孔吸附树脂对黄酮类化合物进行浓缩和纯化可作为前处理的方法。4、研究认为:以甲醇-0.5%HAc作流动相,C18硅胶色谱柱作固定相,283nm的检测波长可以对橘皮提取物的D101大孔树脂纯化物进行选择地分离,得到4种高纯度的物质。

【Abstract】 Contents of this paper consist of optimized extracting factors of flavonoids from citrus peels and methods of separation and purification of single natural compound and stability conditions of extracting matters. The results are showed as follows:1. They have different species and contents of flavonoids in six citrus peels. So it’s essencial to select given breeds in order to obtain the most yield.2. The optimized conditions of extracting flavonoids are studied by different ways such as organic solvents under one atm. As well as under high presure , by supercritical fluid carbon dioxide,limewater under one atm. The purity and rate of production are detected as main parameters. Results showed that extraction by ultrasound under one atm. is cheaper,by organic solvents under high presure is with high rate,by upercutical fluid carbon dioxide is with high purity but low rate. Limewater is the perfecter solvent to extract flavonoid hesperidin. Methanol or ethanol or n-butyl alcohol worked as solvents are without different,of them n-butyl alcohol is the best,ethanol is better .Acetic ether is fit to extract PDF under high pressure.3. The laminar analyses are studied by D101 macroporous resin, strong basicity anion polymeric adsorbent. Seperation by different organic solvent and high speed countercurrent chromtography are studied as well .The rusults showed macroporous resinis is better matter to condense and purify flavonoids except seperation, strong basicity anion polymeric adsorbent adsorbs selectively certein flavonoids . Extracting flavonoids by different polar solvents and testing by HPLC afterwards, it is difficult to separate compounds by simple extraction.4. Separation of flavonoids from citrus peel by HPLC was studied , which worked by methanol-0.5%HAc as solution,C18 resin column as stationary phase. The results showed that whether resolutions or retention time is ideal under chosed conditions. Now it is limited by the weight of flavonoids added to the column.

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