pH区带逆流色谱法分离制备荷梗中O-去甲荷叶碱  

Separation and Preparation of O-nornuciferin from Stems of Nelumbo nucifera Geartn. by pH-zone-refining Counter-current Chromatography

作　　者：宋腾飞[1,2] 许漫丽[3] 巩法强[1,2] 周洪雷[1] 时新刚[2] 王晓[2] 

机构地区：[1]山东中医药大学,山东济南250355 [2]山东省分析测试中心,山东济南250014 [3]中国药科大学,江苏南京211198

出　　处：《辽宁中医杂志》2013年第4期766-768,共3页Liaoning Journal of Traditional Chinese Medicine

基　　金：国家自然科学基金(20872083);山东省科技攻关项目(2010GSF10287);山东省中青年科学家奖励基金(BS2009SW047)

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。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 mmo]/L triethylamine （ TEA ） in organic stationary phase and 5 mmol/L HC1 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 nueifera Geartn.

关 键 词：荷梗 pH区带逆流色谱 O-去甲荷叶碱 

分 类 号：R284[医药卫生—中药学]