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沉淀吸附法提取苦丁茶中的熊果酸
引用本文:任秀莲,魏琦峰,周春山,钟世安,董朝青.沉淀吸附法提取苦丁茶中的熊果酸[J].中南大学学报(自然科学版),2004,35(4):599-603.
作者姓名:任秀莲  魏琦峰  周春山  钟世安  董朝青
作者单位:中南大学,化学化工学院,湖南,长沙,410083
摘    要:依次用碱和酸作沉淀剂,D型树脂作吸附剂,研究了用沉淀-吸附法提取苦丁茶中中熊果酸的工艺.得到的优化条件为:将苦丁茶的乙醇提取液用质量分数为10%的NaOH溶液碱化至pH值约为10.96,过滤除去多酚等杂质,沉淀后,滤液先用体积分数为10%的H2SO4酸化至pH值为4.00,再用相同体积的pH值为4.00的酸性水溶液稀释,得到熊果酸沉淀粗产品;粗产品用甲醇溶解后,将样品溶液pH值调整为7.07,洗脱液pH值调整为11.0,用D型大孔树脂吸附,分步洗脱,收集体积分数为90%乙醇溶液的洗脱液,浓缩结晶得到熊果酸产品.采用高效液相色谱法测得沉淀分离后产品纯度为23.12%,回收率为92.90%;吸附分离后产品纯度为90.23%,回收率为98.02%,总回收率为89.09%.

关 键 词:苦丁茶  熊果酸  大孔吸附树脂  高效液相色谱法
文章编号:1672-7207(2004)04-0599-05
修稿时间:2003年9月15日

Separation and purification of ursolic acid from Ilex Kudingcha by precipitation and adsorption
REN Xiu-lian,WEI Qi-feng,ZHOU Chun-shan,ZHONG Shi-an,DONG Chao-qing.Separation and purification of ursolic acid from Ilex Kudingcha by precipitation and adsorption[J].Journal of Central South University:Science and Technology,2004,35(4):599-603.
Authors:REN Xiu-lian  WEI Qi-feng  ZHOU Chun-shan  ZHONG Shi-an  DONG Chao-qing
Abstract:Sodium hydroxide solution and sulfuric acid solution as precipitation solvents, the process of separation and purification of ursolic acid form Ilex kudingcha was studied. The optimal conditions were obtained as follows: firstly, the alcohol leaching solution was treated to pH 10.011.0 by sodium hydroxide solution with mass fraction 10%, then the polyphenols were removed by filtering, the filtrate was adjusted pH value to 4.0 by sulfuric acid solution with volume fraction 10%, and was diluted by acidic water solution (pH= 4.0), the crude product of ursolic acid was obtained; secondly, it was dissolved by methanol, and adsorbed in macro-porous adsorption resin column, then the resin was eluted fractionally by eluent of alcohol-water and the eluate was collected when pH value of the sample is 6.0(7.0) and pH value of the eluent is 11.0; finally, the product is obtained from the concentrate of 90% alcohol eluent. The products were determined by high performance liquid chromatography (HPLC). The results show that the purity of the product from precipitation separation and adsorption separation is 23.12% and 90.23%, respectively, the recovery is 92.90% and 98.02%, respectively. the total recovery is 89.09%.
Keywords:Ilex Kudingcha: ursolic acid  macro-porous adsorption resin  HPLC
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