大孔树脂纯化乌饭树叶黄酮工艺研究

摘要

In order to purify flavones from Vaccinium Bracteatum Thunb Leaves(VBTL)preliminarily,the static adsorption and de-sorption properties of four resins were compared.The purification technology of flavones from VBTL was investigated by dynamic ad-sorption and desorption experiments.The effect of sample concentra-tion,loading sample volume,ethanol solution for desorption,flow rate of the eluent and volume of eluent on adsorption and desorption rate were studied.In addition,the purification effect was evaluated by removal rate of proteins and polysaccharides and HPLC.The re-sults showed that NKA-II resin had a relatively high rate of adsorp-tion and desorption as well as a shorter adsorption time.NKA-II resin was determined as chromatographic column filler.The optimal purification technology was determined as follows:0.75 mg/mL for sample concentration,2 bed volume (BV)for loading sample volume,50% (v︰v)ethanol solution for desorption,1 mL/min for the flow rate of the eluent and 3 BV for the volume of eluent.HPLC anal-ysis of flavones from VBTL before and after purifying suggested the purity of purified flavones from VBTL improved significantly,and the re-moval rate of proteins and polysaccharides reached 76.32% and 65.45%respectively,with the purity of flavones reaching 48.92%.%为了对乌饭树叶黄酮进行纯化,通过动态吸附与解吸试验,探讨上样体积、上样浓度、上样流速、洗脱剂、洗脱流速以及洗脱体积对乌饭树叶黄酮吸附及解吸效果的影响,然后利用蛋白质和多糖的脱除率以及 HPLC 谱图对纯化效果进行评价.结果表明:NKA-II树脂具有较高的吸附率、解吸率以及较短的吸附时间,确定 NKA-II 树脂作为乌饭树叶黄酮纯化的柱填料,大孔树脂 NKA-II 纯化乌饭树叶黄酮最佳工艺条 件 为:上 样 体 积2.0 BV (柱 体 积),上 样 浓 度0.75 mg/mL,上样流速1 mL/min,洗脱剂为50%(体积分数)的乙醇,洗脱流速1.0 mL/min,洗脱体积3 BV.在该纯化工艺条件下,HPLC表明纯化后乌饭树叶黄酮纯度明显提高,蛋白质脱除率达76.32%,多糖脱除率达65.45%,黄酮纯度达48.92%.