基于HPLC指纹图谱、多指标定量检测及化学计量学的痢泻灵片质量评价

Quality Evaluation of Lixieling Tablets Based on Combinative Methods of HPLC Fingerprint,Quantitative Analysis of Multi-components and Chemometrics Analysis

目的:建立指纹图谱、多指标含量测定与化学计量相结合的痢泻灵片质量评价方法。方法:采用Eclipse plus C18色谱柱(4.6 mm×150 mm,5μm);流动相为乙腈-0.01 mol/L乙酸铵溶液(浓氨试液调pH 8.1)和0.01 mol/L醋酸铵溶液(浓氨试液调pH 8.1),梯度洗脱。以此条件建立10批痢泻灵片的指纹图谱,采用中药色谱指纹图谱相似度评价软件进行相似度评价,并通过SPSS 25.0软件对其进行聚类分析和主成分分析。同时,以此为基础,对痢泻灵片中苦参碱、氧化苦参碱、穿心莲内酯、脱水穿心莲内酯含量进行测定。结果:建立了痢泻灵片的HPLC指纹图谱,共标定出13个共有峰,10批痢泻灵片的相似度为0.921~0.997,苦参碱、氧化苦参碱、穿心莲内酯、脱水穿心莲内酯的含量分别为77.5~302.8μg/g、4.0~171.7μg/g、86.0~160.7μg/g、2.9~40.3μg/g。结论:所建立的痢泻灵片的HPLC指纹图谱和定量分析方法结果准确可靠,可为痢泻灵片质量评价和监管提供依据。

Objective:To establish a quality evaluation method of Lixieling Tablet based on HPLC fingerprints,quantitative analysis of multi-components and chemometrics analysis.Methods:The HPLC fingerprints of Lixieling tablets was performed on Eclipse plus C18 column(4.6 mm×150 mm,5μm),with acetonitrile-0.01 mol/L ammonium acetate solution(using strong ammonia solution to regulate pH in 8.1)and 0.01 mol/L ammonium acetate solution(using strong ammonia solution to regulate pH in 8.1)used as mobile phase A and B for gradient elution,respectively.Similarity evaluation system for chromatographic fingerprint of TCM was used to evaluate the fingerprints and SPSS 25.0 software was used for statistic analysis.With these basises,the contents of matrine,oxymatrine,andrographolide and dehydroandrographolide were determined.Results:The HPLC fingerprints of 10 batches of LiXieLing tablets purchased from the market was established.The similarity was between 0.921-0.997,and 13 common peaks were marked.The content of matrine,oxymatrine,andrographolide and dehydroandrographolide were in the range of 77.5-302.8μg/g,4.0-171.7μg/g,86.0-160.7μg/g and 2.9-40.3μg/g,respectively.Conclusions:The combination methods of HPLC fingerprint and simultaneous determinations of multiple components are accurate,stable and reproducible,which can provide reference for the quality evaluation and administrative supervision of Lixieling tablets.