当归建中汤物质基准特征图谱和多指标成分测定研究

Multi⁃Index Determination and Characteristic Spectrum of Reference Substances of Danggui Jianzhong Decoction

目的建立15批当归建中汤特征图谱及多指标成分含量测定方法,为当归建中汤经典名方的质量控制评价提供参考。方法色谱柱为Waters Symmetry C_(18)色谱柱(4.6 mm×250 mm,5μm);以乙腈(B)⁃0.1%磷酸溶液(A)为流动相,梯度洗脱;流速:1 mL·min^(-1);检测波长为230 nm;柱温35℃;进样量为5μL,建立15批当归建中汤物质基准特征图谱,并使用HPLC测定5种指标成分含量。结果对15批当归建中汤物质基准进行研究,其特征图谱相似度处于0.886~0.996之间,标定了15个共有峰,指认出芍药内酯苷、芍药苷、阿魏酸、甘草苷、肉桂酸、甘草酸6个色谱峰。经方法学考察,5种成分在一定浓度范围内呈良好的线性关系;精密度、稳定性、重复性均符合要求;阿魏酸、肉桂酸、甘草苷、甘草酸、芍药苷的平均加样回收率分别为99.74%、100.28%、100.56%、98.44%、102.25%。以含量测定均值上下浮动30%规定出各指标成分的含量范围,均未出现离散数据(平均值的70%~130%以外)。结论建立的经典名方当归建中汤特征图谱及5个成分的含量测定方法简便、稳定、准确可靠,可用于当归建中汤物质基准的质量控制。

OBJECTIVE To establish the characteristic spectrum and multi⁃components determination of 15 batches of decoction of Danggui Jianzhong,and provide reference for the improvement of its quality control.METHODS High performance liquid chromatography was performed on Waters Symmetry C_(18) column(4.6 mm×250 mm,5μm),and gradient elution was conducted with acetonitrile(B)⁃0.1%phosphoric acid(A)as the mobile phase.The flow rate was 1.0 mL·min^(-1),detection wavelength was set at 225 nm,column temperature was maintained at 35℃,and the injection volume was 5μL.The characteristic spectra of 15 batches of Danggui Jianzhong decoction were established,and the contents of five kinds of index components were determined by the established HPLC method.RESULTS The research on the 15 batches of Danggui Jianzhong decoction showed that the characteristic spectrum similarity was between 0.886⁃0.996,and 15 common peaks were calibrated.Six peaks were identified as albiflorin paeoniflorin,ferulic acid,glycyrrhizin and cinnamic acid,glycyrrhizic acid.According to the methodological investigation,the five components showed a good linear relationship with in a certain concentration range.The precision,repeatability,and stability met the requirements.The average recovery rates of ferulic acid,cinnamic acid,glycyrrhizin,glycyrrhizic acid and paeoniflorin were 99.74%,100.28%,100.56%,98.44%,and 102.25%,respectively.The content range of each index component was defined by the 30%fluctuation of the mean value of the content determination.There was no discrete data(beyond 70%to 130%of the average).CONCLUSION The fingerprint method and the determination method of five components in the traditional Chinese medicine classical prescription named Danggui Jianzhong decoction established in this study are simple,stable,accurate and reliable,and can be used for the quality control of the Danggui Jianzhong decoction.