College of Pharmaceutical Science, Zhejiang University of Technology, Hangzhou 310032, China.
Jinhua Advanced research Institute, Jinhua 321000, China.
J Chromatogr A. 2021 Jun 7;1646:462066. doi: 10.1016/j.chroma.2021.462066. Epub 2021 Mar 15.
Maslinic acid and corosolic acid with high purity were successfully separated from Eriobotrya japonica (Thunb.) leaves by two-step countercurrent chromatographic separation. Two biphasic solvent systems composed of petroleum ether-ethyl acetate-ethanol-water (6:4:5:5, v/v) and petroleum ether-ethyl acetate-ethanol-0.10 mol/L of hydroxypropyl-β-cyclodextrin with pH 7.0 (8:2:3.5:6.5, v/v) were selected according to the partition performance of the main structural isomeric pentacyclic triterpenes. The influences of pH value and concentration of hydroxypropyl-β-cyclodextrin in separation of two isomers were investigated. In first step countercurrent chromatographic separation, a mixture of two target structural isomers (14.12 mg of sample I) was separated from 40.00 mg of a partially purified sample. In second step countercurrent chromatographic separation, maslinic acid and corosolic acid were completely isolated from 12.00 mg of sample I with hydroxypropyl-β-cyclodextrin as aqueous phase additive. The recoveries of the two isomers were over 90%, yielding 5.18 mg of maslinic acid and 5.47 mg of corosolic acid, respectively.
采用两步逆流色谱法成功地从枇杷叶中分离得到高纯度的齐墩果酸和熊果酸。根据主要结构异构型五环三萜类化合物的分配性能，选择了由石油醚-乙酸乙酯-乙醇-水（6:4:5:5，v/v）和石油醚-乙酸乙酯-乙醇-0.10 mol/L 羟丙基-β-环糊精（pH 7.0）（8:2:3.5:6.5，v/v）组成的两相溶剂体系。考察了分离两种异构体时 pH 值和羟丙基-β-环糊精浓度的影响。在第一步逆流色谱分离中，从 40.00mg 部分纯化的样品中分离出两种目标结构异构体（14.12mg 的样品 I）的混合物。在第二步逆流色谱分离中，熊果酸和齐墩果酸完全从 12.00mg 的样品 I 中分离出来，以羟丙基-β-环糊精作为水相添加剂。两种异构体的回收率均超过 90%，分别得到 5.18mg 的齐墩果酸和 5.47mg 的熊果酸。
