Consistency evaluation of commercially Xiaojin Pills using determination of multicomponent contents by HPLC-MS/MS method coupled with chemometrics / 中草药

ABSTRACT

Objective: An HPLC-MS/MS method was established for determination of 10 kinds of components in Xiaojin Pills such as ligustilide, protocatechuic acid, inosine, oleanolic acid, benzoyl neatidine, benzoyl aconitrate, benzoyl aconitine, neaconitine, hypaconitine, aconitine, and combined with cluster analysis, principal component analysis (PCA) and other chemical metrology methods to assess the quality consistency of different batches of Xiaojin Pills from different manufacturers. Methods: The HPLC-MS/MS method was established for the simultaneous determination of 10 active ingredients in Xiaojin Pills. The Agilent Technologies Zorbax Eclipse XDB C18 column (150 mm × 4.6 mm, 5 μm) was used; 0.1% formic acid aqueous solution-acetonitrile as mobile phase; The mass spectrum was scanned by ESI+ multiple reaction monitoring (MRM) mode. And the content analysis was carried out by cluster analysis and principal component analysis, and the difference of the quality of commercially available Xiaojin Pills was evaluated comprehensively. Results: The methodological validation results showed that the linear range of 10 compounds was good (R2 > 0.990 0). The limit of quantification was 0.01-4.49 ng/mL, and the average recovery was 94.82%-104.33%. The results showed that the quality of Xiaojin Pills in a factory was different from others. Benzoyl aconitine, benzoyl aconitine, aconitine and inosine were the main components of classification. The load chart after PCA reduced dimension processing showed that the content of benzoyl neatidine, benzoylthioate, aconitine and inosine were the most distant from the origin, and the difference in content was the main cause of the difference in quality consistency. Conclusion: Considering the poor quality consistency of Xiaojin Pills, the quality control of Aconiti Kusnezoffii Radix and Lonicerae Radix should be strengthened in the production of Xiaojin Pills.