摘要
建立常山中常山碱和异常山碱HPLC同步测定方法,并在此基础上探讨一测多评模式用于这2种生物碱测定的可行性。采用十八烷基键合硅胶色谱柱进行分离,乙腈-水-冰醋酸-三乙胺(9∶91∶0.36∶0.745)为流动相,检测波长225 nm,流速1.0 m L·min^(-1),柱温30℃。结果表明,常山碱和异常山碱分别在10.7~426 ng,10.6~424 ng线性关系良好,平均加样回收率分别为98.33%,100.4%,RSD分别为2.7%,1.8%。在此基础上,以常山碱为内参物,建立了异常山碱对常山碱的相对校正因子与相对保留值。采用一测多评质量评价模式,经一系列方法学考察,最终实现在同一色谱条件下,仅采用常山碱1个对照品就能同时对常山碱和异常山碱2个活性成分进行同步测定。研究结果为一测多评模式在同分异构体测定中的应用起到示范作用。
To develop the HPLC method for simultaneous determination of febrifugine and isofebrifugine in Dichroa febrifuga root, and on the basis of this, the feasibility of quantitative analysis of multi-component by a single-marker （QAMS） model for the determi- nation of the two alkaloids was investigated. The chromatographic separation was performed on an octadecyl bonded silica gel column with mixed solvent consisting of acetonitrile-water-glacial acetic acid-triethylamine （9： 91：0. 36： 0. 745） as mobile phase at a flow rate of 1.0 mL · min^-1. The detection wavelength was set at 225 nm, and the column temperature was set at 30 ℃. The linear range of febrifugine and isofebrifugine were 10. 7-426 ng and 10. 6-424 ng, respectively. Their average recovery were 98.33% （RSD 2. 7% ） and 100. 4% （RSD 1.8% ）, respectively. On the basis of this established method, febrifugine was used as the internal reference sub- stance to calculate the relative correction factors （RCF） and the relative retention values （RRV） of isofebrifugine to febrifugine. Through a series of methodology evaluations, the two alkaloids were simultaneously assayed only by quantitative determination of febri- fugine. This result played the part of demonstration role for the application of QAMS model in the determination of isomers.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2017年第9期1711-1716,共6页
China Journal of Chinese Materia Medica
基金
国家"重大新药创制"科技重大专项(2014ZX09304307001-002-008
2015ZX09501004)
关键词
常山
常山碱
异常山碱
外标法
一测多评法
Dichroafebrifuga
febrifugine
isofebrifugine
external standard method
QAMS
