摘要
目的:对青钱柳叶粗提总三萜化合物进行了纯化,以获得高纯度总三萜化合物,为分离三萜单体奠定基础。方法:大孔树脂动态吸附纯化;超声辅助固液萃取;活性炭脱色;高效预制薄板层析;L-B特征显色鉴定。结果:所选的4种供试大孔树脂中,AB-8对青钱柳三萜化合物具有较好的动态吸附、解吸性能,回收率可达70.89%,纯化后总三萜的纯度可达44.30%,适合于富集和纯化青钱柳叶粗提总三萜;以AB-8树脂动态吸附纯化总三萜,2.75 mg/mL的上样浓度、2 BV/h的上样流速、95%的乙醇洗脱剂、1.0 BV/h的洗脱流速为合适条件;经大孔树脂纯化的总三萜,采用乙酸乙酯进行固液萃取可获得较高的回收率和较好的纯化效果;以活性碳为脱色剂、乙酸乙酯为脱色溶剂微沸处理5 min,可获得较好的脱色效果;精制后的总三萜化合物为淡黄色粉末或片状物,有光泽,纯度可达94.61%。结论:采用AB-8树脂吸附、乙酸乙酯超声辅助固液萃取、活性炭脱色对青钱柳叶粗提总三萜进行纯化,可获得高纯度总三萜化合物。
Objective： In order to get high purity total triterpenoids and reference for separation of single triterpenoid,purification of crude total triterpenoids from Cyclocarya Paliurus leaves was studied in this paper.Methods： Purification by dynamic adsorption of macro-porous resin,solid-liquid extraction assisted by ultrasonic wave,discoloration by activated carbon,High Performance TLC,identification by Libermann-Buehard experiment.Results： Among 4 types of macro-porous resin,AB-8 had a good dynamic adsorption and desorption to the triterpenoids from Cyclocarya Paliurus Leaves and fitted for crude total triterpenoids purification,its recovery percentage was 70.89% and purity of total triterpenoids purified by AB-8 was 44.30%.2.75 mg/mL total triterpenoids in sample,2 BV/h velocity of sample solution,95% ethanol solution and 1 BV/h velocity of strippant were fit for purification by AB-8 resin.Most of total triterpenoids could be extracted by acetic ether from crude total triterpenoids powder purified by AB-8 resin and impurity could be effectively removed by centrifugation.Most of pigments could be effectively removed by adsorption of activated carbon when the total triterpenoids dissolved in acetic ether and kept slight boiling for 5 min.Purity of purified total triterpenoids was 94.61%,and the purified total triterpenoids was powder or sheet,and slight yellow.Conclusion： High purity total triterpenoids from Cyclocarya Paliurus leaves could be produced by dynamic adsorption of macro-porous resin,solid-liquid extraction assisted by ultrasonic wave and discoloration by activated carbon.
出处
《食品科技》
CAS
北大核心
2011年第2期161-165,共5页
Food Science and Technology
基金
江西省科技支撑计划项目(2009BSB09100)
江西省自然科学基金项目(2007GZN0214)
关键词
青钱柳
总三萜
精制
Cyclocarya paliurus
total triterpenoids
purification
