摘要
研究了从山楂叶中纯化熊果酸的柱层析工艺。静态吸附结果表明,X-5、NKA和AB-8树脂的吸附率分别为91.32%,72.28%和41.19%;以90%乙醇为洗脱剂,X-5、NKA和AB-8树脂的洗脱率分别为83%,70%,87%。静态实验表明X-5树脂具有较好的吸附解吸性能。动态实验优化了在X-5树脂中的流速、上样液的熊果酸浓度和上样体积。结果表明,流速为3BV/h(BV为倍量体积),上样液的熊果酸浓度为0.304mg/mL,上样体积为3BV为最优上样条件。动态洗脱中采用梯度洗脱方式,结果表明在90%的乙醇洗脱下,熊果酸纯度达93.21%。对层析工艺制备的熊果酸进行结晶处理,所获得的熊果酸纯度为98.61%,与熊果酸标准品的红外光谱一致。
The column chromatography technique for the preparative isolation of ursolic acid from Hawthorn leaves was investigated. Adsorption efficiency of X-5, NKA and AB-8 were 91.32%, 72.28% and 41.19%, respectively; desorption efficiency of X-5, NKA and AB-8 were 83%, 87%, , 70% using 90% alcohol elution, respectively. The results showed that X-5 resin was the best in static adsorption and elution. The flow rate, content of ursolic acid and volume for X-5 column were optimized, and the optimum conditions were flow rate 3BV/h, content of ursolic acid 0.304mg/mL and volume 3BV. A proper step-gradient elution was used, which resulted in an efficient isolation： the purity of ursolic acid was 93.21%. The purity of ursolic acid reached 98.61% by the recrystallization procedure, and the IR spectrum of the ursolic acid was consistent with that of the standard sample.
出处
《广州化学》
CAS
2006年第2期23-27,共5页
Guangzhou Chemistry
关键词
山楂叶
熊果酸
大孔吸附树脂
分离纯化
hawthorn leaves, ursolic acid, macroporous resin, separation and isolation
