摘要
目的:建立加味葛根颗粒的指纹图谱,测定其中6种成分的含量,并进行正交偏最小二乘判别法分析(OPLS-DA)。方法:采用HPLC法,色谱柱为Tech Mate-C18柱,流动相为乙腈-0.05%磷酸溶液(梯度洗脱),检测波长为254 nm,柱温为35℃,流速为1 mL·min^(-1)。采用《中药色谱指纹图谱相似度评价系统》2012年版进行相似度评价,确定共有峰,并测定其中6种成分的含量;采用SIMCA 14.0软件进行OPLS-DA分析,并利用分析变量重要性投影值(VIP)筛选影响其质量的标志物。结果:10批加味葛根颗粒共有14个共有峰,相似度均>0.9;共指认了6个色谱峰并分别测定了含量,各成分在考察范围内线性良好,r值在0.999 0~0.999 9之间。OPLS-DA筛选得到了6个VIP>1的共有峰(峰13、峰7、峰12、峰2、峰8、峰9),经对照品指认了其中3个差异性标志物(肉桂酸、原儿茶酸、芍药苷)。结论:结合多元统计分析,建立的指纹图谱和含量测定方法准确、稳定、可行,可用于加味葛根颗粒的质量控制。
Objective:To establish the fingerprint of Jiawei Gegen Granules,determine the contents of six components,and conduct orthogonal least squares criterion(OPLS-DA)analysis.Methods:The contents of six components were determined by HPLC with Tech Mate-C18 column applying the mobile phase of acetonitrile-0.05%phosphate solution in gradient elution.The flow rate was 1 mL·min^(-1),the detection wavelength was set at 254 nm,and the column temperature was 35℃.The similarity was evaluated with“TCM Chromatographic Fingerprint Similarity Evaluation System”(2012 Edition)by determining common peaks and the contents of six components.Finally,OPLS-DA analysis with SIMCA 14.0 software and the analytical variable importance projection(VIP)values were used to screen the markers.Results:There were 14 peaks in 10 batches of Jiawei Gegen Granules with similarity above 0.9.A total of six chromatographic peaks were identified and determined.The calibration curve of each component was linear in the test ranges with r values of 0.9990~0.9999.OPLS-DA screening obtained six common peaks ( peaks 13,7,12,2,8,9) with variable importance projections ( VIP) > 1,and three of them( cinnamic acid,protocatechuic acid,paeoniflorin) could be served as differential markers. Conclusion: Combinedwith multivariate statistical analysis,the established fingerprint map and content determination method are accurate,stable,and feasible,which can be used for the quality control of Jiawei Gegen Granules.
作者
李文莉
李军鸽
朱凯
王永春
楚云杰
LI Wen-li;LI Jun-ge;ZHU Kai;WANG Yong-chun;CHU Yun-jie(The Affiliated Hospital of Changchun University of Chinese Medicine,Changchun 130117,China;Changchun University of Traditional Chinese Medicine,Changchun 130117,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2024年第9期934-941,共8页
Chinese Journal of New Drugs
基金
吉林省科技发展计划项目(20220401063YY)。
关键词
加味葛根颗粒
指纹图谱
含量测定
聚类分析
Jiawei Gegen Granules
fingerprint
content determination
cluster analysis