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目的建立对荷叶生物碱进行分离的pH区带逆流色谱方法。方法溶剂系统为叔丁基甲醚-甲醇-水(4∶1∶5),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800 r/min、体积流量1.5 mL/min、检测波长254 nm条件下进行分离制备。结果从2.18 g荷叶提取物中一次分离得到N-去甲荷叶碱110 mg、O-去甲荷叶碱420 mg、荷叶碱310 mg和莲碱190 mg 4种生物碱,质量分数均大于98%;各化合物通过HPLC、MS和1H-NMR进行了化学结构鉴定。结论 pH区带逆流色谱法是一种快速高效的分离纯化荷叶生物碱的方法。
Objective To establish a pH zone countercurrent chromatography method for the separation of alkaloids from lotus leaf. Methods The solvent system was tert-butyl methyl ether-methanol-water (4: 1: 5). Triethylamine (10 mmol / L) was added as the stationary phase in the upper phase and hydrochloric acid (5 mmol / L) Off, the host speed 800 r / min, the volume flow rate of 1.5 mL / min, detection wavelength 254 nm under the conditions of preparation. Results Four alkaloids of norethindrone 110 mg, o-norefine 420 mg, nuciferine 310 mg and naline 190 mg were isolated from 2.18 g lotus leaf extract at one time. More than 98%. The chemical structure of each compound was identified by HPLC, MS and 1H-NMR. Conclusion The pH-zone countercurrent chromatography is a rapid and efficient method for the isolation and purification of lotus leaf alkaloids.