基于含量测定和化学计量分析的消渴灵片质量标准研究

目的:建立13个厂家111批消渴灵片中黄连的6个生物碱、丹皮酚等多指标性成分含量测定方法,并结合主成分分析及聚类分析等化学计量学方法对其进行质量评价研究。方法:采用HPLC-UV法建立6个黄连生物碱类成分(非洲防己碱、表小檗碱、盐酸药根碱、盐酸黄连碱、盐酸巴马汀、盐酸小檗碱)、丹皮酚的含量测定方法及通过Chempatten化学计量学软件对不同生产企业的消渴灵片进行系统比较和评价。结果:建立消渴灵片的含量测定方法,测定了其中7个成分的含量,各个成分均能达到基线分离,进样量分别在6.05~249、9.29~226、5.94~195、11.0~283 ng、9.94~267、55.4~1847、23.576~589.410 ng范围内与峰面积呈良好的线性关系,平均回收率分别为90.0%、84.8%、91.9%、90.3%、93.1%、93.0%、92.3%,符合方法验证要求。同时,化学计量统计体现了所建立的含量测定方法可以对不同生产企业生产的样品进行区分。结论:本实验所建立的多指标含量测定方法简单易行,准确性、稳定性和重复性良好,综合主成分分析和聚类分析,可为消渴灵片质量标准提供参考。

Standardization of Xiaokeling tablets based on assay and stoichiometric analysis

Objective:To establish a stoichiometric method for the quantitative evaluation of the active principle ingredients(API)in Rhizoma Coptidis,six alkaloids and paeonol,in 111 batches of Xiaokeling tablets produced by 13 manufactures.Methods:The assay method of alkaloids in Rhizoma Coptidis(afriline,epiberberine,jatrorrhizine hydrochloride,coptidine hydrochloride,palmatine hydrochloride and berberine hydrochloride)and paeonol in Xiaokeling tablets was established by HPLC-UV processed by the software Chempatten.Results:7 components were separated well on baseline.The injection ranges were 6.05-249 ng,9.29-226 ng,5.94-195 ng,11.0-283 ng,9.94-267 ng,55.4-1847 ng and 23.576-589.410 ng,respectively,which were in good linear with the peak areas.The average recoveries met methodological requirements at 90.0%,84.8%,91.9%,90.3%,93.1%,93.0% and 92.3%,respectively.It indicated that stoichiometric assays were applicable for sample tracings.Conclusion:The above-mentioned method is proved to be simple,accurate,stable and repeatable,and showing referential significance for the quantitative standardization of Xiaokeling tablets.