【摘要】 目的:建立pH区带逆流色谱法(pH-zone refining counter-current chromatography)分离制备荷梗中O-去甲荷叶碱的方法。方法:溶剂系统为石油醚-乙酸乙酯-甲醇-水(3∶7∶1∶9),上相添加三乙胺(10 mmol/L)作为固定相,下相添加盐酸(5 mmol/L)为流动相进行洗脱,在主机转速850 r/min、体积流量2 mL/min、检测波长272 nm条件下进行分离制备。结果:从2.10 g荷梗生物碱粗提物中一次分离得到53 mg O-去甲荷叶碱,纯度大于98%,通过MS、1H-NMR和13C-NMR进行了化学结构鉴定。结论:pH区带逆流色谱法是分离纯化荷梗中O-去甲荷叶碱的一种快速高效的分离方法。更多还原

【Abstract】 Objective:A novel method for the separation of O-nornuciferin from the stems of Nelumbo nucifera Geartn.by pH-zone-refining counter-current chromatography(pH-ZRCCC) was carried on.Methods:The two-phase solvent system composed of light petroleum-ethyl acetate-methanol-water(3∶ 7∶ 1∶ 9),10 mmol/L triethylamine(TEA) in organic stationary phase and 5 mmol/L HCl in aqueous mobile phase.The upper phase was used as the stationary phase,while the lower phase as the mobile phase.In one-step elution under the conditions of a flow rate of 2 mL/min,850 r/min and the effluent was detected at 254 nm.Results:From 2.10 g of the crude extract,53 mg O-nornuciferin was obtained and with the purity over 98% as determined by HPLC.The structure of the isolated compound was identified by ESI-MS,1H-NMR and 13C-NMR.Conclusion:The present pH-ZRCCC method may be applied to the purification of O-nornuciferin from the stems of Nelumbo nucifera Geartn.更多还原