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目的:分离纯化赤雹根中的dubioside F,鉴定结构并测定不同产地赤雹根中dubioside F的含量。方法:通过硅胶柱色谱分离纯化,以CHCl3-Me OH-H2O(14∶7∶1)为洗脱剂,得到单体化合物,根据其理化性质和波谱数据,鉴定该单体化合物为dubioside F;再以分离得到的dubioside F为对照品,测定不同产地赤雹根药材中dubioside F的含量。采用Discovery-C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-水(24∶76),流速1.0 m L·min-1,检测波长200 nm。结果:dubioside F在0.98~24.5μg线性关系良好(r=1),平均回收率96.96%,RSD 1.1%。结论:首次对赤雹根中单体皂苷类成分(dubioside F)进行含量测定,测定方法简便、快速、可靠。不同产地种植、野生的赤雹根药材dubioside F的含量,分别以吉林省和龙市、河北省宽城县出产的为最高。可为进一步的赤雹根药材质量控制的研究提供依据。
OBJECTIVE: To isolate and purify dubioside F from red hail roots, identify the structure and determine the content of dubioside F in red hail roots from different habitats. METHODS: The compounds were separated and purified by silica gel column chromatography with CHCl3-Me OH-H2O (14: 7: 1) as eluent. The compounds were identified as dubioside F by their physical and chemical properties and spectral data. The isolated dubioside F was used as a reference substance to determine the content of dubioside F in red hail roots from different areas. The mobile phase was acetonitrile-water (24:76) with a flow rate of 1.0 mL · min-1 on a Discovery-C18 column (4.6 mm × 250 mm, 5 μm). The detection wavelength was 200 nm. Results: The linearity of dubioside F at 0.98 ~ 24.5μg was good (r = 1), with an average recovery of 96.96% and a RSD of 1.1%. Conclusion: The content of monomeric saponins (Dubioside F) in hail hail is determined for the first time. The determination method is simple, rapid and reliable. The content of dubioside F in wild and cultivated red hail roots was highest in Kaohsiung and Kaohsiung provinces in Jilin Province and Kuancheng County in Hebei Province. It can provide the basis for the further research on quality control of red hail roots.