黄芪甲苷含量测定方法的优化及对不同产地、不同等级黄芪中黄芪甲苷含量分析

Optimization of determination methods of astragaloside Ⅳ and analysis of contents of astragaloside Ⅳ in different origin and grade

建立一种快速、准确的黄芪甲苷含量测定方法,通过测定87批不同产地及不同等级黄芪药材中黄芪甲苷含量,对不同产地黄芪甲苷含量限度采用ROC曲线分析,同时结合化学计量学对不同等级黄芪甲苷含量进行比较。采用HPLC-ELSD测定,使用Vensil MP C18色谱柱(4. 6 mm×250 mm,5μm),以乙腈-水(32∶68)为流动相,流速1 m L·min-1,柱温25℃,ELSD参数:气体流速2. 5 L·min-1,漂移管加热温度105℃,增益值4. 0。结果表明改进方法在样品前处理中不仅避免了耗材质量不稳定导致回收率不高问题,而且测定值高于药典方法,具有节省时间、重复性好等特点。ROC曲线分析表明山西仿野生芪特等、一等黄芪甲苷含量与甘肃移栽芪无明显差异,二等、三等、四等黄芪甲苷含量显著高于甘肃移栽芪。等级比较结果表明山西仿野生芪黄芪甲苷含量与等级呈显著负相关,而甘肃移栽芪无相关性。该研究为黄芪质量等级标准提供研究基础。

A rapid and accurate method for determination of astragalosideⅣwas established,which was further applied to determine the contents of astragalosideⅣin 87 batches of different origin and different grade of Astragali Radix.The ROC curve was used to analyze the contents of astragalosideⅣin different origin.Simultaneous contents of astragalosideⅣin different grade were compared with chemometrics.HPLC-ELSD method was used to determine the contents of astragalosideⅣ.A Vensil MP C18 column(4.6 mm×250 mm,5μm)was used with acetonitrile-water(32∶68)as the mobile phase at a flow rateof 1 m L·min-1.The column temperature was 25℃with ELSD parameters as follows:gas flow rate was 2.5 L·min-1,the drift tube heating temperature was set to 105℃,and the gain value was 4.0.The optimized method avoided the problem that the consumable quality unstable and the recovery rate was not high.The contents determined by the optimized method were higher than the pharmacopoeia method,with less time and high recovery rate.The ROC curve analysis showed that there was no significant difference of contents of astragalosideⅣbetween the top grade of Shanxi wild-simulated Astragali Radix top and the first grade of Gansu cultivated Astragali Radix.The contents of astragalosideⅣin the second,third and fourth grade of Shanxi wild-simulated Astragali Radix was significantly higher than those of produced from Gansu.There was a significant negative correlation between the contents of astragalosideⅣand grade in Shanxi Astragali Radix.While there was no correlation for Gansu Astragali Radix.This study provided the basis for the quality grade standard of Astragali Radix.