基于特征图谱结合化学计量学和一测多评法的北刘寄奴配方颗粒质量评价  

Quality evaluation of Siphonostegiae Herba formula granules based on specific chromatograms combined with chemometrics and quantitative analysis of multi-components with a single-marker

作　　者：张京华 吴娜娜 吕亚男 曹桂云 董晓弟 林永强 李金鑫 孟兆青 ZHANG Jinghua;WU Nana;LYU Yanan;CAO Guiyun;DONG Xiaodi;LIN Yongqiang;LI Jinxin;MENG Zhaoqing(Shandong Hongjitang Pharmaceutical Group Co.,Ltd.,Shandong Province Technical Innovation Center of Traditional Chinese Medicine Treatment of Respiratory Diseases,Jinan 250103,China;Shandong Institute for Food and Drug Control,Jinan 250101,China)

机构地区：[1]山东宏济堂制药集团股份有限公司,山东省中医药治疗呼吸系统疾病技术创新中心,山东济南250103 [2]山东省食品药品检验研究院,山东济南250101

出　　处：《中草药》2024年第14期4722-4734,共13页Chinese Traditional and Herbal Drugs

基　　金：山东省重点研发计划重大科技创新工程项目(2021CXGC010511);泉城“5150”引才倍增计划(2021年)。

摘　　要：目的建立HPLC法特征图谱结合化学计量学和一测多评法(quantitative analysis of multi-components with a single-marker method,QAMS)的方法,对北刘寄奴(Siphonostegiae Herba,SH)配方颗粒(formula granules,SHFG)进行质量评价。方法利用15批北刘寄奴标准汤剂(SH standard decoctions,SHSD)建立HPLC特征图谱,并对指认的成分采用QAMS法测定含量。基于标准汤剂出膏率、指标成分含量及转移率,研究配方颗粒与标准汤剂的一致性,同时以特征图谱相似度评价法、聚类分析及主成分分析(principal component analysis,PCA)、QAMS法对配方颗粒进行质量评价。结果15批标准汤剂和8批配方颗粒特征图谱相似度均>0.9,确定了12个共有峰,指认咖啡酸、夏佛塔苷、对香豆酸、阿魏酸、毛蕊花糖苷、异毛蕊花糖苷、木犀草素、芹菜素8个成分。聚类分析及PCA可将15批标准汤剂和8批配方颗粒分成2类,C厂家2批配方颗粒(S22、S23)单独为一类。15批北刘寄奴标准汤剂出膏率为11.70%~21.73%,咖啡酸、夏佛塔苷、对香豆酸、阿魏酸、木犀草素、芹菜素、毛蕊花糖苷、异毛蕊花糖苷质量分数分别为0.18~0.60、0.21~3.83、0.64~2.36、0.05~1.03、0.54~2.52、0.23~0.63、8.97~24.62、5.78~16.80 mg/g,其从饮片到标准汤剂转移率分别为23.28%~42.17%、26.73%~47.73%、21.98%~39.62%、24.00%~42.48%、8.85%~14.88%、18.54%~30.86%、19.12%~30.56%、26.87%~44.35%。A厂家3批北刘寄奴配方颗粒(S16~S18)出膏率、指标成分含量及转移率与同批次饮片制备的标准汤剂接近,且均在质量标准规定范围内;B、C厂家5批北刘寄奴配方颗粒(S19~S23)8种指标成分含量均在标准汤剂按制成量折算后含量范围内。结论所建立的特征图谱结合化学计量学及QAMS法,可系统全面地评价北刘寄奴配方颗粒的质量,为北刘寄奴配方颗粒的工艺研究、质量控制以及临床应用提供参考。Objective To establish the HPLC specific chromatography combined with chemometric analysis and quantitative analysis of multi-components with a single-marker method(QAMS) for the quality evaluation of Beiliujinu(Siphonostegiae Herba) formula granules(SHFG).Methods The HPLC specific chromatography of 15 batches of Siphonostegiae Herba standard decoctions(SHSD)was established,and the contents of identified components were determined by the QAMS method.Based on the extraction rates,index component contents,and transfer rates of the standard decoctions,the consistency of formula granules with the standard decoctions was studied.The quality of SHFG was evaluated by similarity analysis,cluster analysis,principal component analysis,and the QAMS method.Results The similarity between specific chromatograms of 15 batches of SHSD and eight batches of SHFG were more than 0.9,12 common peaks were calibrated,and eight components(caffeic acid,schaftoside,p-coumaric acid,ferulic acid,verbascoside,isoacteoside,luteolin and apigenin) were identified.Cluster analysis and principal component analysis can divide 15 batches of SHSD and eight batches of SHFG into two categories,and two batches of SHFG(S22,S23) from manufacturer C were classified as a single category.The extraction rates of 15 batches of SHSD were 11.70%—21.73%,the contents of caffeic acid,schaftoside,p-coumaric acid,ferulic acid,luteolin,apigenin,verbascoside and isoacteoside were 0.18—0.60,0.21—3.83,0.64—2.36,0.05—1.03,0.54—2.52,0.23—0.63,8.97—24.62,5.78—16.80 mg/g and the transfer rates of these components from the herbal pieces to SFSD were 23.28%—42.17%,26.73%—47.73%,21.98%—39.62%,24.00%—42.48%,8.85%—14.88%,18.54%—30.86%,19.12%—30.56%,26.87%—44.35%.The extract rates,index component contents,and transfer rates of index compounds in three batches of SHFG(S16—S18)from manufacturer A were close to the standard decoction prepared from the same batch of medicinal materials,and were all within the scope of the quality standard.The conte

关 键 词：北刘寄奴 标准汤剂 配方颗粒 HPLC 特征图谱 一测多评法 化学计量学 主成分分析 咖啡酸 夏佛塔苷 对香豆酸 阿魏酸 毛蕊花糖苷 异毛蕊花糖苷 木犀草素 芹菜素 

分 类 号：R283.6[医药卫生—中药学]