Ma Jie, Chen Qianliang, Lai Daowan, Sun Wenji, Zhang Tianyou, Ito Yoichiro
Biomedicine Key Laboratory of Shaanxi Procvince, Northwest Univesity, Xi'an, 710069, China.
J Liq Chromatogr Relat Technol. 2010 Jan 1;33(4):563-571. doi: 10.1080/10826070903574659.
Coupled with evaporative light scattering detection, high-speed countercurrent chromatography was successfully applied for the first time to separation and purification of four triterpene saponins including esculentoside A, B, C and D from roots of Radix Phytolaccae. The separation was performed with an optimized two-phase solvent system composed of chloroform-methanol-water (4:4:2, v/v) using the lower phase as the mobile phase at a flow rate of 1.5 ml/min,. From 150 mg of crude extract 46.3 mg of esculentoside A, 21.8 mg of esculentoside B, 7.3 mg of esculentoside C, and 13.6 mg of esculentoside D were obtained at purities of 96.7%, 99.2%, 96.5% and 97.8%, respectively, as determined by HPLC analysis. The structures of the four triterpene saponins were identified by ESI-MS,(1)H NMR and (13)C NMR.
结合蒸发光散射检测，高速逆流色谱首次成功应用于从商陆根中分离纯化包括商陆皂苷甲、乙、丙和丁在内的四种三萜皂苷。采用氯仿 - 甲醇 - 水（4:4:2，v/v）组成的优化两相溶剂系统进行分离，以下层相作为流动相，流速为1.5 ml/min。从150 mg粗提取物中分别获得了46.3 mg商陆皂苷甲、21.8 mg商陆皂苷乙、7.3 mg商陆皂苷丙和13.6 mg商陆皂苷丁，经HPLC分析测定，纯度分别为96.7%、99.2%、96.5%和97.8%。通过电喷雾电离质谱、氢核磁共振和碳核磁共振对这四种三萜皂苷的结构进行了鉴定。
