高速逆流色谱结合蒸发光散射检测法从商陆根中分离纯化三萜皂苷
Separation and purification of triterpene saponins from roots of Radix phytolaccae by high-speed countercurrent chromatography coupled with evaporative light scattering detection.
作者信息
Ma Jie, Chen Qianliang, Lai Daowan, Sun Wenji, Zhang Tianyou, Ito Yoichiro
机构信息
Biomedicine Key Laboratory of Shaanxi Procvince, Northwest Univesity, Xi'an, 710069, China.
出版信息
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。
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