固精麦斯哈片的HPLC特征图谱与化学模式识别研究  

Characteristic chromatogram and quality evaluation of Gujing Maisiha tablets by HPLC coupled with chemometrics

作　　者：常道潇 耿小秀 李辉 温锦荣 王震 CHANG Dao-xiao;GENG Xiao-xiu;LI Hui;WEN Jin-rong;WANG Zhen(Shaanxi Shengde Tailin Biological Safety Technical Testing Co.,Ltd.,Xi'an 710065,China;Xi'an Wanlong Pharmaceutical Co.,Ltd.,Xi'an 710119,China)

机构地区：[1]陕西盛德泰林生物安全技术检测有限公司,西安710065 [2]西安万隆制药股份有限公司,西安710119

出　　处：《药物分析杂志》2024年第11期1875-1884,共10页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立固精麦斯哈片HPLC特征图谱,并运用化学模式识别进行质量评价研究。方法:采用Welch Xtimate C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-0.1%甲酸(B)为流动相进行梯度洗脱(0~10 min,5%A→15%A;10~20 min,15%A;20~40 min,15%A→40%A;40~65 min,40%A→70%A;65~66 min,70%A→90%A;66~80 min,90%A;80~81 min,90%A→5%A;81~85 min,5%A),流速1.0 mL·min-1,检测波长254 nm,柱温35℃。建立固精麦斯哈片特征图谱,并进行相似度评价、聚类分析、主成分分析和正交偏最小二乘判别分析。结果:建立了固精麦斯哈片的特征图谱,从10批样品中共确定28个共有峰,指认了其中7个成分,分别为没食子酸、绿原酸、苦番红花素、异槲皮苷、西红花苷-Ⅰ、西红花苷-Ⅱ、丁香酚。10批固精麦斯哈片特征图谱与对照图谱的相似度结果均大于0.98,聚类分析按照欧氏距离为10可将样品分为2类,与主成分分析结果一致。正交偏最小二乘判别分析筛选出5个差异性成分,分别来自丁香、玫瑰花和熏鲁香药材。结论:本次建立的固精麦斯哈片HPLC特征图谱方法高效可行,重复性好,可为本品质量标准提高研究提供参考。Objective:To establish the HPLC characteristic chromatogram for Gujing Maisiha tablets,and evaluate the quality using chemical pattern recognition.Methods:The Welch Xtimate C_(18)column(250 mm×4.6 mm,5μm)was used and the mobile phases were acetonitrile(A)and 0.1%formic acid(B)in gradient elution(0-10 min,5%A→15%A;10-20 min,15%A;20-40 min,15%A→40%A;40-65 min,40%A→70%A;65-66 min,70%A→90%A;66-80 min,90%A;80-81 min,90%A→5%A;81-85 min,5%A).The detection wavelength was 254 nm.The column temperature was 35℃and the flow rate was 1.0 mL·min~(-1).Gujing Maisiha tablets were analyzed to construct characteristic chromatogram.The quality of Gujing Maisiha tablets was assessed through similarity evaluation,cluster analysis,principal component analysis(PCA),and partial least squares discriminant analysis(PLS-DA).Results:The characteristic chromatogram of Gujing Maisiha tablets was established,which contained the twenty-eight distinct peaks,and seven compounds identified as gallic acid,chlorogenic acid,picrocrocin,isoquercitrin,crocin-Ⅰ,crocin-Ⅱ,eugenol.The similarities for the ten batches of Gujing Maisiha tablets were more than 0.98,with no significant difference observed.Cluster analysis segregated the samples into two distinct groups according to the Euclidean distance of 10,which was consistent with the results of PCA analysis.PLS-DA analysis screened out five components from Flos Caryophylli,Rosae Rugosae Flos,Olibanum that may cause differences between samples.Conclusion:The method of HPLC characteristic chromatogram of Gujing Maisiha tablets is effective,feasible and reproducible,which can provide reference for the study of quality standard of this product.

关 键 词：固精麦斯哈片 特征图谱 相似度评价 化学模式识别 没食子酸 西红花苷-Ⅰ 西红花苷-Ⅱ 丁香酚 

分 类 号：R917[医药卫生—药物分析学]