油茶茶籽壳中茶皂素分离纯化及结构分析的研究

Separation,Purification and Structural Analysis of Tea Saponin from Camellia oleifera Seed Shell

以油茶茶籽壳为原料,采用乙醇提取法对其皂素类物质进行粗提取,HPD-100大孔树脂吸附法对茶皂素粗提物进行纯化,利用紫外光谱和超高效液相色谱-质谱法对纯化样品进行鉴定。实验结果表明,最佳提取工艺参数为:料液比1∶15,乙醇体积分数75%,提取温度70℃,提取时间120 min,其最高提取率达25.58%。粗提物经HPD-100大孔树脂纯化,30 mg/mL粗提液上样,水和20%乙醇洗去极性大的杂质,80%乙醇溶液洗脱出茶皂素,茶皂素纯化得率为48.63%,纯度提高1.38倍。该工艺操作简单,适合于茶皂素的分离。纯化茶皂素通过紫外光谱和液质联用检测,结果显示该样品为52种茶皂素单体的混合物并得到了其在质谱中的裂解规律。

Tea saponin was extracted from the Camellia oleifera seed shell by ethanol and purified by HPD-100 macroporous resin.Ultraviolet-vis spectroscopy(UV)and ultra-performance liquid chromatography-mass spectrometry(LC-MS)were used for identification of the purified samples.The results indicated that the optimum conditions of extraction were as follows:solid-liquid ratio of 1∶15 g/mL,ethanol concentration of 75%,extraction temperature of 70℃and extraction time of 120 min.The highest extraction rate of tea saponin was 25.58%.The crude extract was purified by HPD-100 macroporous resin,30 mg/mL crude extract was loaded,water and 20%ethanol were eluted to remove polar impurities,and 80%ethanol solution was eluted to remove tea saponin.The purification yield of saponin was 48.63%,the purity was improved 1.38 times.The purified tea saponin sample was detected by UV and LC-MS.The purified sample was a mixture of 52 kinds of tea saponin monomers,and its cracking rule in mass spectrometry was obtained.