黄芪中黄芪甲苷含量测定的新方法探讨

New Method for Determination of Astragaloside Ⅳ in Astragali Radix

目的:探讨黄芪中黄芪甲苷含量测定的新方法的可行性。方法:通过对文献涉及的黄芪中黄芪甲苷测定方法的梳理,采用一种黄芪甲苷测试的新方法,即"回流碱化衍生法"。开展了含量测定预试,并对新方法与2015年版《中国药典》方法(简称药典法)所测的不同批次黄芪中黄芪甲苷的含量数据进行了比较。结果:回流碱化衍生法测定黄芪甲苷的方法学符合相关规定,且测定的黄芪中黄芪甲苷的含量高于药典法。标准曲线为Y=1. 315X+6. 311 2(r=0. 999 7,n=6,线性范围0. 044 6~8. 92μg),日内精密度、日间精密度的RSD分别为0. 5%,0. 6%,重复性试验RSD 1. 2%,48 h稳定性试验的RSD2. 1%,回收率试验的RSD 2. 0%。回流碱化衍生法、药典法测定的16批黄芪饮片中黄芪甲苷的质量分数分别为0. 371%,0. 203%,0. 315%,0. 218%,0. 386%,0. 221%,0. 353%,0. 192%,0. 303%,0. 197%,0. 373%,0. 188%,0. 361%,0. 114%,0. 349%,0. 112%;0. 243%,0. 152%,0. 214%,0. 168%,0. 274%,0. 157%,0. 221%,0. 133%,0. 203%,0. 141%,0. 257%,0. 132%,0. 238%,0. 084%,0. 242%,0. 096%。结论:回流碱化衍生法可用于黄芪饮片中黄芪甲苷的含量测定,较药典法操作起来更加简便、黄芪甲苷衍生物的转化效率更好、可重复性更好。该方法可以为形成快速、科学、准确的黄芪甲苷含量测定方法提供参考。

Objective: To study on the feasibility of a new method for determination of astragaloside Ⅳ in Astragali Radix. Method: By summarizing the literatures about the method for determining the content of astragaloside Ⅳ in Astragali Radix and analyzing the results of the preliminary test,a new method for preparing a test solution of astragaloside was established,named " Reflow alkalization derivatization method ". The content determination test was carried out,and the content data of astragaloside Ⅳ in different batches of Astragali Radix measured by the pharmacopoeia method were compared with that by the Reflow alkalization derivatization method.Result: The new method for the determination of astragaloside Ⅳ conformed to the corresponding regulations. The content of astragaloside Ⅳ in astragali radix determined by the new method was higher than that by the pharmacopoeia method. The standard curve was Y = 1. 315 X + 6. 311 2( r = 0. 999 7,n = 6,linear range is 0. 044 6-8. 92 μg). The RSDs of intraday precision and daytime precision were 0. 5% and 0. 6%,respectively.The RSD of the repetitive experiment was 1. 2%. The RSD of the 48 h stability test was 2. 1%,and the RSD of the recovery test was 2. 0%. The contents of astragaloside Ⅳ in 16 batches of Astragali Radix determined by Reflow alkalization derivatization method and pharmacopoeia method were 0. 371%,0. 203%,0. 315%,0. 218%,0. 386%, 0. 221%, 0. 353%, 0. 192%, 0. 303%, 0. 197%, 0. 373%, 0. 188%, 0. 361%, 0. 114%,0. 349%, 0. 112%;0. 243%, 0. 152%, 0. 214%, 0. 168%, 0. 274%, 0. 157%, 0. 221%, 0. 133%,0. 203%,0. 141%, 0. 257%, 0. 132%, 0. 238%, 0. 084%, 0. 242%, and 0. 096%. Conclusion: The Reflow alkalization derivatization method can be used to determine the content of astragaloside Ⅳ in Astragali Radix. This method is simpler to operate than the pharmacopoeia method, and the conversion efficiency of astragalus glycosides derivatives is better and reproducible. This method can provide reference for the formation of a fast,scientific and accurate method for the determination of astragalus Ⅳ.