目的 建立HPLC一测多评法(quantitative analysis of multi-components by single-marker,QAMS)法联合化学计量学对利胆石颗粒质量控制的方法。方法 采用HPLC-QAMS对3个厂家的10批利胆石颗粒中双去甲氧基姜黄素、去甲氧基姜黄素、姜黄素、柚皮芸香苷、橙皮苷、川陈皮素、3,5,6,7,8,3',4'-七甲氧基黄酮、橘红素、香附烯酮、圆柚酮和α-香附酮含量进行同时检测;再利用SPSS 26.0、SIMCA 14.1软件对上述指标的QAMS法计算数据进行层次聚类分析(hierarchical cluster analysis,HCA)、主成分分析(principal component analysis,PCA)及偏最小二乘-判别分析(partial least squares-discriminant analysis,PLS-DA),综合评价利胆石颗粒质量及标志性成分。结果 11种成分分别各自范围内线性关系良好(r>0.999 3);平均加样回收率在96.87%~100.08%,RSD在0.66%~1.56%;HPLC-QAMS法所测结果与外标法(ESM)无显著性差异;通过化学计量学分析,10批利胆石颗粒聚为3类,同一厂家聚为一类,不同厂家的质量存在一定的差异,柚皮芸香苷(VIP=1.745)、橙皮苷(VIP=1.470)、香附烯酮(VIP=1.350)和姜黄素(VIP=1.188)可能是影响利胆石颗粒产品质量差异的标志物。结论 所建立的HPLC-QAMS法多指标成分定量控制及化学计量学模式识别专属性强,可用于利胆石颗粒质量控制和综合评价。

Objective To establish a method for quality control of Lidanshi Granules (利胆石颗粒,LG) by HPLC-quantitative analysis of multi-components by single-marker (QAMS) combined with chemometrics. Methods HPLC-QAMS was used to simultaneously detect the contents of bisdemethoxycurcumin,demethoxycurcumin,curcumin,narirutin,hesperidin,nobiletin,3,5,6,7,8,3',4'-heptamethoxyflavone,tangeretin,cyperenone,nootkatone and α-cyperone in 10 batches of LG from three manufacturers.SPSS 26.0 and SIMCA 14.1 software were used to conduct hierarchical cluster analysis (HCA),principal component analysis (PCA) and partial least squares-discriminant analysis (PLS-DA) on the QAMS calculation data of the above indexes,so as to comprehensively evaluate the quality and symbolic components of LG.Results The linear ranges of 11 components were good (r>0.999 3).The average recoveries were 96.87%-100.08%,RSDs were 0.66%-1.56%.There was no significant difference between HPLC-QAMS and external standard method (ESM).Through chemometrics analysis,10 batches of LG were clustered into three categories,and the same manufacturer was clustered into one category.There was certain difference in the quality of different manufacturers,narirutin (VIP=1.745),hesperidin (VIP=1.470),cyperenone (VIP=1.350) and curcumin (VIP=1.188) might be the differential markers affecting the quality of LG.Conclusion Establishment of HPLC-QAMS multi-index component quantitative control and application of chemometric pattern recognition are specific,which can be used for quality control and comprehensive evaluation of LG.

R286.02

全国中药特色技术传承人才培训项目(国中医药人教函[2019]43号T20194828003)