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建立了薄层色谱图像分析定量-高速逆流色谱法从吴茱萸甲醇提取物中快速分离制备吴茱萸碱、吴茱萸次碱、吴茱萸卡品碱3个化合物的方法。采用数码相机对HSCCC溶剂系统上下相中的目标化合物进行TLC图像采集,使用积分软件OPSIA计算各溶剂系统对应的K值,筛选出最佳溶剂系统正己烷-乙酸乙酯-甲醇-水(3:2.5:3.5:2,V/V)。取上相为固定相,下相为流动相,检测波长为254 nm,在主机转速860 r/min、流动相流速1.5 mL/min的条件下,一次性从300 mg样品中分离制备得到经1H-NMR和13C-NMR确证的吴茱萸碱(15.3mg)、吴茱萸次碱(10.1 mg)、吴茱萸卡品碱(20.7 mg),纯度分别为93.6%,97.3%和95.1%(HPLC法)。
A method was established for the rapid separation of three compounds of evodiamine, rutaecarpine and evodiamine by quantitative-high speed countercurrent chromatography from Evodia rutaecarpa methanol extract by thin-layer chromatography. TLC images of the target compounds in the upper and lower phases of HSCCC solvent system were collected by digital camera. The corresponding K values of each solvent system were calculated by the integral software OPSIA. The optimum solvent system was n-hexane-ethyl acetate-methanol-water (3: 2.5: 3.5: 2, V / V). The upper phase was the stationary phase and the lower phase was the mobile phase. The detection wavelength was 254 nm. Under the condition of the host rotation speed of 860 r / min and the mobile phase flow rate of 1.5 mL / min, The contents of evodiamine (15.3 mg), rutaecarpine (10.1 mg) and evodiamine (20.7 mg) were confirmed by -NMR and 13C-NMR, respectively. The purity was 93.6%, 97.3% and 95.1%, respectively.