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目的建立高速逆流色谱(HSCCC)技术高效快速地分离制备益母草中益母草碱的方法。方法单因素实验优化益母草碱的提取工艺,而后考察不同的HSCCC溶剂体系,根据分配系数(K),确定溶剂体系为醋酸乙酯-正丁醇-水(3∶2∶5),以其上相为固定相,下相为流动相,转速850 r/min,体积流量2.2 mL/min,检测波长为277 nm,对益母草样品进行HSCCC分离。结果益母草正丁醇萃取部位通过HSCCC可分离得到益母草碱,该方法成功应用于益母草粗提物中益母草碱的分离:1次HSCCC运行可从2.48 g益母草70%乙醇粗提物(益母草碱质量分数为3.01%)中分离得到68 mg益母草碱,质量分数为96.2%,得率为2.74%。结论建立的方法可高效分离纯化益母草中的益母草碱,为得到高纯度的益母草碱提供了制备技术。
OBJECTIVE To establish a high-speed countercurrent chromatography (HSCCC) technique for the rapid and efficient separation of Leonurine from Leonurus. Methods The single factor experiment was used to optimize the extraction process of Leonurine, and then different HSCCC solvent systems were investigated. Based on the partition coefficient (K), the solvent system was determined to be ethyl acetate - n-butanol - water The phases were stationary phase, the lower phase was mobile phase, the rotational speed was 850 r / min, the volume flow rate was 2.2 mL / min and the detection wavelength was 277 nm. The samples of Motherwort were separated by HSCCC. Results Leonurine extracted from Leonurus amylol extract could be fractionated by HSCCC, and the method was successfully applied to the isolation of Leonurine from the crude extract of Leonurus. The results showed that one run of HSCCC could be performed from 2.48 g of 70% Ethanol extract of Leonurus Was 3.01%) to obtain 68 mg of Leonurus, with a mass fraction of 96.2% and a yield of 2.74%. Conclusion The established method can efficiently separate and purify Leonurine from the motherwort and provide the preparation technology for the high purity of Leonurine.