赤雹根中Dubioside F的分离纯化及含量测定

Purification and Determination of Dubioside F in Tuber of Thladiantha dubia

摘要:

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-MeOH-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,5 μm),流动相乙腈-水(24:76),流速1.0 mL·min^-1,检测波长200 nm. 结果: dubioside F在0.98~24.5 μg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.

Abstract:

Objective: The aim of this study was to purify and determine the content of dubioside F in the tuber of Thladiantha dubia from different habitats by HPLC Method: Dubioside F was purified by column chromatograph with silica gel(CHCl₃-MeOH-H₂O 14:7:1)and identified through physicochemical properties and spectral analysis. To determine the content of dubioside F in the tuber of T. dubia from different habitats by HPLC:A Discovery-C₁₈ (4.6 mm×250 mm, 5 μm) column was used with the mobile phase of acetonitrile-water (24:76). The DAD detector was set at 200 nm. Result: Dubioside F showed good linearity (r=1) within test ranges(0.98-24.5 μg). The average recovery was 96.96%, with RSD of 1.1%. Conclusion: This method was well validated in good precision, repeatability and sensitivity. The most abundant dubioside F in the tuber of T. dubia in different cultivated habitats was from Helong of Jilin rovince;while the most abundant dubioside F in the tuber of T. dubia in different natural habitats is from Kuancheng of Hebei province. This method was successfully applied to quantify dubioside F in the tuber of T. dubia.