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黄芪有效组分的提取分离及结构鉴定
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摘要
黄芪为豆科植物,以根入药。多年来一直以黄芪甲苷为其质量控制指标,药理学研究结果表明,黄芪中产生药效的有效成分还有黄芪黄酮、黄芪皂苷和黄芪多糖等。本课题为提高这三类化学成分的提取率,采用酶解法首先处理黄芪药材,然后再进行黄芪黄酮、黄芪皂苷和黄芪多糖的提取分离,达到了预期的实验目的。研究确定的实验结果:采用正交实验法确定了在pH4.6、纤维素酶用量0.8%、温度60℃、酶解120min的条件下,对黄芪药材进行提取前处理,使得黄芪多糖、黄芪总黄酮和黄芪总苷的提取率都有大幅度的提高。其中黄芪多糖的提取率比未酶解的黄芪提高了300%以上。酶解后的黄芪药材采用80%乙醇回流提取法提取总黄酮和总皂苷,再用组合分离技术进行分离纯化:聚酰胺吸附总黄酮后的水洗脱液流经D101大孔吸附树脂吸附总皂苷,达到分离纯化总黄酮和总皂苷的目的,二者的提取率分别为4.79%和1.26%,纯度依次为58.0%和79.3%。进一步利用碱水解法从总皂苷中富集纯化得到了两个单体化合物,经结构鉴定分别为AstragalosideⅢ和AstragalosideⅣ。经乙醇提取后的黄芪药渣挥尽乙醇,按固液比1:11的量加入蒸馏水,回流提取3次,每次75 min,总糖提取率可达33.6%。采用超滤法分段收集黄芪总多糖,其分子量大于50000Da的多糖约占12.23%,在10000~50000Da之间的多糖占68.25%,而小于10000 Da的占19.52%。纤维素酶技术的应用使黄芪资源得到了充分的利用,有效组分的研究扩大了临床药效指标。酶解-膜分离-色谱技术的联合应用,为黄芪有效组分的工业化生产提供了科学依据。
The radix astragali is the leguminous plant,is used as medicine by the root.For many years continuously take AstragalosideⅣas its quality control target,The Pharmacology findings indicated,In the radix astragali produces the drug efficacy effective component also to have the radix astragali flavanone,saponin and polysaccharide and so on。This topic to enhance these three kind of chemical composition the extraction rate,Uses the cellulose hydrolysis first to process the radix astragali,Then carries on the radix astragali flavanone,the saponin and the polysaccharide extraction separation again,Has served the anticipated experiment purpose。Research definite experimental result:Used the orthogonal experiment method to determine in pH4.6,the cellulase amount used 0.8%,temperature 60℃,under the enzymolysis 120min condition,carried on the extraction before the radix astragali to process, causes the radix astragali polysaccharide,the total flavanone and the total glucoside extraction rate has the large scale enhancement.And the radix astragali polysaccharide's extraction rate compared the enzymolysis radix astragali not to enhance above 300%。After enzymolysis radix astragali uses 80%ethyl alcohol backflow extraction process to withdraw the total flavanone and the total saponin,uses the combination isolation technique to carry on the separation purification again:After polymide adsorbs the total flavanone the water eluent to flow through the D101 macroporous resin adsorb the total saponin,and the separation to purify the total flavanone and the total saponin,the two's extraction rate is 4.79%and 1.26%, the purity is 58.0%and 79.3%。using the lye solution from the total saponin to obtain two compound,was AstragalosideⅢand AstragalosideⅣ。Wield the completely ethyl alcohol after the ethyl alcohol extraction's radix astragali dregs of medical decoction,joins the distilled water according to the liquid-solid compared to the 1:11 quantity,the backflow withdraws 3 times,each time 75 min,the total sugar extraction rate is 33.6%.Uses the ultrafiltration partition collection radix astragali total polysaccharide,its molecular weight is bigger than 50000Da the polysaccharide to approximately compose 12.23%,accounts for 68.25%between the 10000~50000Da polysaccharide,while is smaller than 10000Da accounts for 19.52%.
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