动态轴向压缩色谱制备高纯度断氧化马钱子苷的研究

Isolation of High-Purity Secoxyloganin from Flos Lonicera Japonica by Industrial Dynamic Axial Compression Preparative Chromatography

目的:本研究旨在建立动态轴向压缩色谱法分离制备高纯度断氧化马钱子苷的方法。方法:金银花70%乙醇提取液先经大孔吸附树脂除杂富集后,采用动态轴向压缩色谱柱分离,以正相硅胶为填料,二氯甲烷-甲醇系统为洗脱剂,对断氧化马钱子苷进行精制纯化,分别运用HPLC、1H-NMR、13C-NMR和HR-ESI-MS对断氧化马钱子苷进行含量测定和结构表征。结果:产品经分析确定为断氧化马钱子苷,质量分数达98.76%。结论:采用动态轴向压缩工业色谱法制备断氧化马钱子苷的方法操作简便、快速、高效,为制备高纯度的断氧化马钱子苷提供了一条新途径。

This study was aimed to establish an industrial chromatographic separation technology of high-purity secoxyloganin. The 70% alcohol extract of Flos L. japonica was separated and concentrated by macroporous resin and industrial chromatography. Normal phase silica gel was taken as solid phase, and methylene chloride-methanol system as eluent for the dynamic axial compression column. The determination and characterization of secoxyloganin was detected by HPLC, 1^H-NMR, 13^C-NMR and HR-ESI-MS. The results showed that the content of secoxyloganin reached to 98.76%. It was suggested that the industrial chromatographic separation technology of secoxyloganin was convenient, rapid and efficient, which provided a new method for the preparation of high-purity ecoxyloganin.