红豆杉叶氯仿萃余相中黄酮类化合物的分离纯化

Separation and Purification of Flavonoids from Remainder Extracts of Taxus Chinensis Leaves

建立1种制备性分离南方红豆杉叶氯仿萃余相中黄酮类化合物的方法。将氯仿萃取南方红豆杉叶醇提物剩余相用AB-8型大孔树脂层析柱进行初分离,收集浓缩样品,用聚酰胺层析柱分离纯化浓缩液,硝酸钠-硝酸铝显色,紫外分光光度法定量测定总黄酮含量。优化的AB-8型大孔树脂分离紫杉黄酮工艺条件为:样品进样体积60 mL(1 BV),解吸液为80%乙醇,解吸体积180 mL,在此条件下浸膏紫杉黄酮含量达到20.65%;优化的聚酰胺层析柱分离紫杉黄酮化合物工艺条件为:样品进样体积30 mL(1 BV),解吸液为70%乙醇,解吸液体积120 mL,在此条件下浸膏黄酮含量达63.05%。红豆杉叶醇提液的氯仿剩余相中总黄酮含量为2.83%。AB-8型大孔树脂层析与聚酰胺层析联合分离使总黄酮百分含量提高60.22倍。

In the present work, the preparative separation of flavonoids from Taxus mairei （chinensis） remainder ex-tracts free of taxoids using macroporous resins and polyamide resin was studied. The performance of adsorption and des-orption characteristics of six macroporous resins including HZ-816, X-5, AB-8, HZ-801, NKA-9 and S-8 had been evaluated. The research results indicated that AB-8 resin was the most appropriate for the separation of flavonoids. Col-umn packed with AB-8 resin was used to perform dynamic adsorption and desorption tests to optimize the separation process. The optimum parameters for adsorption were as follows： processing volume： 60mL （1 BV）, desorption solution： ethanol-water （80：20,V/V）, processing volume： 180mL, the percentage of flavonoids in the eluent is 20.65%. The opti-mum parameters for polyamide resin are as follows： processing volume： 30mL （1 BV） for desorption： ethanol-water （70： 30,F/F）, processing volume： 120 mL, the percentage of flavonoids increased to 63.05%. Using AB-8 resin and polyamide column to separate and purify flavonoids from Taxus mairei （chinensis） remainder extracts free of taxoids could increase the percentage of flavonoids to 60.22%.