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目的:利用pH区带逆流色谱法(pH-zone-refining countercurrent chromatography)对三尖杉生物碱进行分离。方法:将三氟乙酸加入乙酸乙酯-石油醚-水(3∶1∶4)溶剂系统的上相(固定相)作为保留剂,用含10%氨水、中性和含三氟乙酸的下相(流动相)依次进行梯度洗脱,取得了较好的分离效果。结果:1次分离可进样500 mg,分离得到4组三尖杉生物碱,其中2组经核磁共振(NMR)分析为三尖杉碱和乙酰三尖杉碱。经HPLC分析,2种生物碱的纯度分别为95.4%和98.9%。结论:pH区带逆流色谱法是一种较好的三尖杉生物碱分离方法。
Objective: To use the pH-zone-refining counter current chromatography to separate the harringtonine alkaloids. Method: Trifluoroacetic acid was added to the upper phase (stationary phase) of the ethyl acetate-petroleum ether-water (3:1:4) solvent system as a retentate with 10% aqueous ammonia, neutral and trifluoroacetic acid. The phase (mobile phase) was sequentially eluted with a gradient, and a good separation effect was obtained. RESULTS: A total of 500 mg could be injected in one separation. Four groups of harringtonine alkaloids were isolated. Two groups were analyzed by NMR to harringtonine and acetyl harringtonine. By HPLC analysis, the purity of the two alkaloids was 95.4% and 98.9%, respectively. Conclusion: pH zone counter-current chromatography is a better method for the separation of alkaloids from harringtonine.