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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: To establish a method for the preparation of o-norefine in peduncle by pH-zone refining counter-current chromatography. Methods: The solvent system was petroleum ether - ethyl acetate - methanol - water (3: 7:1:9). Triethylamine (10 mmol / L) ) Was used as eluent. The mobile phase was centrifuged at 850 r / min, the volume flow rate was 2 mL / min and the detection wavelength was 272 nm. Results: 53 mg of O-demetaormene was isolated from the crude extract of 2.10 g stalk alkaloids and the purity was more than 98%. The chemical structure was identified by MS, 1H-NMR and 13C-NMR. CONCLUSION: The pH-zone countercurrent chromatography is a rapid and efficient method for the isolation and purification of o-naloxine in peduncle.