百部止咳糖浆中黄酮类成分的HPLC指纹图谱化学模式识别分析

Chemical pattern recognition analysis of flavonoids in Baibu Zhike syrup by HPLC fingerprint

目的:建立百部止咳糖浆中黄酮类成分的HPLC指纹图谱、多组分含量测定和化学模式识别相结合的分析与评价方法,为其质量标准提升提供理论基础。方法:采用Agilent ZORBAX Eclipse XDB C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,流速为1.0 mL·min^(-1),柱温为30℃,检测波长为280 nm,进样体积10μL。建立百部止咳糖浆样品黄酮类成分HPLC指纹图谱,使用中药色谱指纹图谱相似度评价系统、Origin 2021 PRO和SPSS 26.0软件进行指纹图谱分析、相似度评价、黄酮类成分含量测定、主成分因子分析和聚类分析。结果:26批次样品的相似度在0.70~0.99,共确认12个共有峰,并指认出7个色谱峰,分别为芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷、黄芩苷、汉黄芩苷、川陈皮素,并对其中柚皮苷、橙皮苷、新橙皮苷、黄芩苷、汉黄芩苷进行含量测定。进行主成分因子分析,提取的2个公因子分别为黄芩质量因子和陈皮、枳壳质量因子。因子分析结果:小儿百部止咳糖浆(XETJ)所含黄酮类成分得分高于复方百部止咳糖浆(FFTJ);FFTJ中的生产企业A在黄酮类成分方面综合质量表现最佳;XETJ中的生产企业G在黄酮类成分方面质量表现更佳。聚类分析结果表明,当分类距离为15时,所有样品被分为3类。结论:本研究方法简便可靠、重复性良好,可用于百部止咳糖浆中黄酮类成分的质量分析与评价。

Objective:To establish a quality analysis and evaluation method of flavonoids in Baibu Zhike syrup by combining HPLC fingerprint,multi-component content determination,and chemical pattern recognition analysis,to provide a theoretical basis for improving its quality standards.Methods:Chromatographic separation was conducted on Agilent ZORBAX Eclipse XDB C_(18)column(250 mm×4.6 mm,5μm)in a gradient program.The mobile phase consisted of 0.1%aqueous formic acid and acetonitrile,and the column temperature was 30℃.The flow rate was 1.0 mL·min^(-1),the detection wavelength was 280 nm,and the injection volume was 10μL.The fingerprint spectra of flavonoids in Baibu Zhike syrup samples were established and the TCM chromatography fingerprint spectrum,Origin 2021 PRO and SPSS 26.0 software were applied for similarity evaluation,flavonoid content determination,principal component factor analysis,and cluster analysis.Results:The similarity of 26 batches of samples ranged from 0.70 to 0.99,and a total of 12 common peaks were confirmed.Seven chromatographic peaks were identified,namely narirutin,naringin,hesperidin,neohesperidin,baicalin,wogonoside and nobiletin.The contents of naringin,hesperidin,neohesperidin,baicalin,and wogonoside were determined.The results of principal component factor analysis showed that the extracted two common factors were the quality factor of Scutellariae Radix and the quality factor of Citri Reticulatae Pericarpium and Aurantii Fructus,respectively.For factor analysis,XETJ scored higher than FFTJ in terms of flavonoid components,enterprise A in FFTJ had the best overall quality performance in terms of flavonoid components,and enterprise G in XETJ performs better in overall quality of flavonoid components.The clustering analysis results indicated that when the classification distance was 15,all samples were divided into three categories.Conclusion:This research method is simple,reliable and repeatable,and can be used for the quality analysis and evaluation of flavonoids in Baibu Zhike syrup.