摘要
目的:建立寒喘祖帕颗粒HPLC指纹图谱及多指标成分定量分析方法,结合化学模式识别技术对其进行质量评价。方法:通过优化样品前处理及色谱检测条件,建立寒喘祖帕颗粒HPLC指纹图谱和含量测定条件。色谱柱为YMC-Pack ODS-A柱(250 mm×4.6 mm,5μm,12 nm),以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,检测波长220 nm,柱温30℃,体积流量1.0 mL·min^(-1)。采用聚类分析(HCA)、主成分分析(PCA)、正交偏最小二乘-判别分析(OPLS-DA)对17批寒喘祖帕颗粒进行质量评价。结果:寒喘祖帕颗粒HPLC指纹图谱及含量测定方法学考察结果均符合测定要求,获得25个共有峰,指认了8个色谱峰;17批样品的相似度均>0.90,样品间一致性及稳定性良好;由HCA可知,17批样品可大致聚成3类;PCA从25个共有峰中提取了3个主成分,通过OPLS-DA筛选了16号峰(芦丁)、3号峰(没食子酸)、15号峰、23号峰、24号峰(甘草酸)和7号峰(绿原酸)6个引起不同批次寒喘祖帕颗粒质量差异的主要标志性成分;8个定量成分线性关系均良好(r≥0.9994),平均加样回收率98.0%~99.1%,RSD均<2.0%。结论:建立的寒喘祖帕颗粒HPLC指纹图谱结合多指标成分定量方法,专属性强、简便、准确,可为其整体质量控制和品质评价提供参考依据。
Objective:To establish the HPLC fingerprint and multi-component quantitative analysis of Hanchuang Zupa granules,and evaluate the quality of multiple batches of Hanchuang Zupa granules by chemical pattern recognition technology.Methods:The sample pretreatment conditions and chromatographic analysis conditions of Hanchuang Zupa granules were optimized,and the optimal HPLC fingerprint and multi-component quantitative analysis method were established as follows:stationary phase was YMC-Pack ODS-A column(250 mm×4.6 mm,5μm,12 nm)was adopted,and the mobile phase was acetonitrile-water(containing 0.1%phosphoric acid)with gradient elution,the detection wavelength was 220 nm,the column temperature was 30℃,the flow rate was 1.0 mL·min^(-1).Hierarchical cluster analysis(HCA),principal components analysis(PCA)and orthogonal partial least squares-discriminant analysis(OPLS-DA)were applied to evaluate the quality of 17 batches of Hanchuang Zupa granules.Results:Methodological investigation of HPLC fingerprint and content determination were well verified and met the analysis requirements.A total of 25 common peaks were obtained by full peak matching,and eight of them were identified by comparing with the retention time of mixed reference substances.The similarities of 17 batches of samples were above 0.90,which showed good consistency and stability between the samples.Seventeen samples could be classified into three clusters.Three principal components from 21 common peaks were extracted by PCA.Six quality differential compounds were presented in the fingerprints by OPLS-DA,including rutoside,gallic acid,ammonium glycyrrhizinate,chlorogenic acid and so on.The resolution and linear relationship of eight components in quantitative analysis were good.The average recovery rates were 98.0%-99.1%with RSD≤2.0%.Conclusion:In this study,the qualitative analysis of HPLC fingerprint and quantitative analysis of multiple index components is specific,simple and accurate,which can provide a reference for the quality control and quality evaluation of Hanchuang Zupa granules.
作者
魏培
曹春泉
钱淼
朱瑞娟
孙新堂
WEI Pei;CAO Chun-quan;QIAN Miao;ZHU Rui-juan;SUN Xin-tang(Food and Drug Technology Department of Shandong Vocational Animal Science and Veterinary College,Weifang 261061,China;Pharmacy Department of Heze University,Heze 274000,China)
出处
《药物分析杂志》
CSCD
北大核心
2024年第12期2127-2137,共11页
Chinese Journal of Pharmaceutical Analysis
关键词
寒喘祖帕颗粒
高效液相色谱指纹图谱
化学模式识别
定量分析
质量控制
Hanchuang Zupa granules
high-performance liquid chromatography fingerprints
chemical pattern recognition
quantitative analysis
quality control
作者简介
通信作者:孙新堂,Tel:(0536)3086321,E-mail:sdmysxt@163.com;第一作者:魏培,Tel:(0536)3086430,E-mail:108584969@qq:com。
