摘要:
为了确定枸杞叶黄酮的最佳纯化工艺及纯化后产物的结构和含量,本文比较了AB-8、DM301、NKA-9、HPD-100、HP-20、D101六种大孔吸附树脂的吸附解析性能,并选取吸附性能与解吸效果最好的树脂对上样条件及洗脱条件进行研究,考察上样浓度、上样液pH、上样流速、以及洗脱剂的浓度、流速、用量对洗脱性能的影响。采用紫外可见光谱(UV-Vis),傅立叶变换红外光谱(FT-IR)、高效液相色谱(HPLC)对纯化物组成和结构进行分析。结果表明,D101型大孔吸附树脂的吸附性能与解吸效果最好,其最佳纯化工艺为:上样浓度3.728 mg/mL,上柱液pH6,上样流速2 mL/min,以70%乙醇为洗脱液,洗脱流速2 mL/min,洗脱液用量3.5 BV。以此工艺纯化枸杞叶黄酮粗提物,其总黄酮含量由355.05 mg/g提高到809.89 mg/g,提高了2.28倍。经紫外可见光谱(UV-Vis)扫描分析纯化产物具有黄酮类化合物C6-C3-C6的基本结构;经傅立叶变换红外光谱(FT-IR)扫描分析其多种特征官能团包括C=O、羟基、酚羟基、甲氧基以及甲基较粗提物更为突出;经高效液相色谱(HPLC)检测,该纯化产物中芦丁、绿原酸、槲皮素、咖啡酸、对香豆酸、山奈酚、阿魏酸的含量依次为:179.45、60.92、3.14、6.35、2.66、2.45、1.38 mg/g。
Abstract:
In order to determine the best purification process of Lycium barbarum leaves flavone,confirm the structure and contents of the product after purification. Comparing the adsorption and desorption performance of six macro porous adsorption resins including AB-8,DM301,NKA-9,HPD-100,HP-20 and D101,and selecting the best one to research the condition of sample and elution,investigation on pH of sample,concentration of sample,sample flow rate,and the concentration,dosage,flow rate of elution. The composition and structure of the purified compounds were analyzed by UV-Vis,FT-IR and HPLC. The results showed that the D101 macro porous adsorption resin had the best adsorption performance and desorption effect. The optimal purification process was as follows:The concentration of the upper sample was 3.728 mg/mL,the pH of the upper column was 6,and the flow rate of the upper sample was 2 mL/min. The eluent of 70% ethanol was used,the flow rate was 2 mL/min,and the amount of the eluent was 3.5 BV. Under the conditions,the total flavonoid content increased from 355.05 mg/g to 809.89 mg/g with a 2.28 fold increase. The detection for UV-Vis showed that the purified product had the basic structure of flavonoid C6-C3-C6. FT-IR test showed that the multiple characteristic functional groups including C=O,hydroxyl,phenol hydroxyl,methyl and methyl were more prominent than the crude extract. By HPLC,the contents of rutin,chlorogenic acid,quercetin,caffeic acid,p-coumaric acid,kaempferol and ferulic acid in the purified product were 179.45,60.92,3.14,6.35,2.66,2.45 and 1.38 mg/g respectively.
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