宫瘤消胶囊HPLC指纹图谱及多成分定量分析  

HPLC Fingerprint and Multi-component Quantitative Analysis of Gongliuxiao Capsules

作　　者：于凤蕊 林林 许丽丽 徐兴燕 李军 崔巧红 林永强 YU Feng-rui;LIN lin;XU Li-li;XU Xing-yan;LI Jun;Cui Qiao-hong;LIN Yong-qiang(Shandong Engineering Laboratory for Standard Innovation and Quality Evaluation of TCM,Shangdong Engineering Research Center for Generic Technologies of Traditional Chinese Medicine Formula Granules,Shandong Institute for Food and Drug Control,Jinan 250101,China;Shandong Danhong Pharmaceutical Co.,Ltd.,China;Shandong Shenzhou Buchang Pharmaceutical Co.,Ltd.,Heze 274000,China)

机构地区：[1]山东省食品药品检验研究院,山东省中药标准创新与质量评价工程实验室,中药配方颗粒共性技术山东省工程研究中心,山东济南250101 [2]山东丹红制药有限公司,山东菏泽274000 [3]山东步长神州制药有限公司,山东菏泽274000

出　　处：《食品与药品》2024年第6期481-487,共7页Food and Drug

基　　金：山东省重点研发计划(重大科技创新工程)项目(编号:2022CXGC010511);泉城产业领军人才支持计划创新团队项目(编号:MRJT2105)。

摘　　要：目的建立宫瘤消胶囊高效液相色谱(HPLC)指纹图谱和多成分含量测定方法,并结合化学计量学方法进行质量评价。方法采用Kromasil-100-5-C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈(A)-0.2%磷酸溶液(B)为流动相,梯度洗脱(0~25 min,10%A→55%A;25~26 min,55%A→90%A;26~35 min,90%A),流速为1.0 ml/min,柱温为35℃,检测波长:310 nm,15~35 min切换为245 nm。结果建立了宫瘤消胶囊HPLC指纹图谱,标定16个共有峰,指认了10个共有峰,分别为没食子酸、新绿原酸、绿原酸、1,2,3,4,6-五没食子酰葡萄糖、4-香豆酸、芹菜素-7-葡萄糖苷、苯甲酰芍药苷、丹皮酚、莪术呋喃二烯酮和α-香附酮,并进行了定量研究,各项方法学考察结果均符合测定要求。19批样品指纹图谱相似度均大于0.92;聚类分析将19批样品按生产年份聚为2类,表明不同年份的样品间存在一定的质量差异;主成分分析提示1,2,3,4,6-五没食子酰葡萄糖、4-香豆酸、丹皮酚、莪术呋喃二烯酮、峰15和α-香附酮对其质量影响较大,可作为指标性成分。结论建立的HPLC指纹图谱和多成分含量测定方法可为宫瘤消胶囊质量标准提高和修订提供参考,单纯依靠指纹图谱相似度评价有一定局限性,需结合化学计量学方法进行综合评价。Objective To establish the HPLC fingerprint and multi-component quantitative analysis method of Gongliuxiao Capsules,and combined with chemometrics,to evaluate the quality of the drug.Methods The analysis was carried out on a Kromasil 100-5-C_(18)(250 mm×4.6 mm,5μm)column,using acetonitrile(A)and 0.2%phosphoric acid solution(B)as mobile phase of gradient elution(0-25 min,10%A→55%A;25-26 min,55%A→90%A;26~35 min,90%A).The flow rate was 1.0 ml/min,and the column temperature was 35℃.The detection wavelength was set at 310 nm,and switched to 245 nm from 15 to 35 min.Results HPLC fingerprint of Gongliuxiao Capsules was established,16 common peaks were found,and 10 common peaks were identified and quantitatively studied,including gallic acid,neochlorogenic acid,chlorogenic acid,1,2,3,4,6-pentagalloylglucose,4-coumaric acid,apigenin-7-glucoside,benzoylpaeoniforin,paeonol,furanodienone andα-cyerone.All methodological investigation results met the testing requirements.The similarity of fingerprints of 19 batches of samples were greater than 0.92.Cluster analysis grouped 19 batches of Gongliuxiao Capsules samples into 2 categories based on production years,indicating that there were certain quality differences between the samples of different years.Principal component analysis suggested that 1,2,3,4,6-pentagalloylglucose,4-coumaric acid,paeonol,furanodienone,peak 15,andα-cyerone had significant impact on the quality and could be used as index components.Conclusion The established HPLC fingerprint and multi-component quantitative analysis method can provide reference for the improvement and revision of the quality standard of Gongliuxiao Capsules.Quality evaluation only using fingerprint analysis has certain limitations and needs to be combined with chemometric methods for comprehensive evaluation.

关 键 词：宫瘤消胶囊 指纹图谱 含量测定 聚类分析 主成分分析 

分 类 号：R284.1[医药卫生—中药学]