清热解毒口服液指纹图谱的建立及质量评价模式研究  

Quality evaluation of Qingrejiedu oral liquid based on fingerprints combined with chemometrics

作　　者：陈荣 钟水生 王亚琼 张超 陈卫 CHEN Rong;ZHONG Shui-sheng;WANG Ya-qiong;ZHANG Chao;CHEN Wei(Suzhou Institute for Drug Control,Suzhou Jiangsu 215104,China)

机构地区：[1]苏州市药品检验检测研究中心,苏州215104

出　　处：《药物分析杂志》2023年第12期2154-2164,共11页Chinese Journal of Pharmaceutical Analysis

基　　金：江苏省药品监督管理局科研计划课题(202128)。

摘　　要：目的:基于清热解毒口服液HPLC指纹图谱,建立质量评价方式,考察各厂家样品质量情况。方法:采用Diomonsil Plus C18色谱柱(250 mm×4.6 mm,5μm),以甲醇-0.4%甲酸水溶液为流动相,梯度洗脱,流速为1 mL·min^(-1),柱温为35℃,检测波长为238、280(29 min,238→280 nm),建立指纹图谱,结合化学计量学及统计学技术,进行初步质量评价。结果:清热解毒口服液指纹图谱共标定30个共有峰,全部进行归属,其中确证成分26个(根据对照品比对确证22个,根据QTOF/MS和文献确证4个),结合化学计量学中聚类分析和主成分分析,可将不同厂家样品予以区分,质量较好的厂家样品栀子苷、龙胆苦苷以及金银花的酚酸类成分含量明显更高,而质量差的厂家样品只有黄芩苷含量与其他厂家无明显差异。结论:该方法能宏观评价各厂家样品的优劣,将指纹图谱和化学计量学以及统计学技术联用是较为适宜、全面的质量评价手段。Objective:To establish a quality evaluation method to investigate the quality of samples from different manufacturers based on the HPLC fingerprints of Qingrejiedu oral liquid.Methods:The analysis was performed on a Diomonsil Plus C_(18)column(250 mm×4.6 mm,5μm)with methanol-0.4%formic acid aqueous solution as mobile phases in gradient elution,1 mL·min^(-1)as flow rate and 35℃as column temperature.The detection wavelength were 238 nm(0-29 min)and 280 nm(29-90 min).The HPLC fingerprints were established to evaluate the quality of samples from different manufacturers combined with chemometrics and statistics.Results:Thirty chromatographic peaks were recognized as common peaks in the Qingrejiedu oral liquid fingerprints,all of which were attributed,and 26 components were confirmed.Among them 23 components were confirmed by comparison with reference substances and 4 components were identified by QTOF/MS and literature.Combining with cluster analysis and principal component analysis,the samples from different manufacturers could be distinguished.The contents of geniposide,gentiopicroside and phenolic acids,in the samples from manufacturers with better quality were significantly higher than those of the samples from manufacturers with poor quality.Only the content of baicalin had no obvious difference between them.Conclusion:This method can be used to macroscopically evaluate the quality of the samples from different manufacturers.The combination of fingerprint and stoichiometry or statistics technology is a suitable and comprehensive quality evaluation method.

关 键 词：清热解毒口服液 指纹图谱 化学计量学 黄芩苷 栀子苷 龙胆苦苷 

分 类 号：R917[医药卫生—药物分析学]