基于临床验方的六金颗粒制备及质量标准研究  

Study on Preparation Technology and Quality Standard of Liujin Granules Based on Clinical Experience

作　　者：罗毅 秦金淼 张荣飞 刘子夜 曹桂云 姚元成 孟兆青 容蓉[1] LUO Yi;QIN Jinmiao;ZHANG Rongfei;LIU Ziye;CAO Guiyun;YAO Yuancheng;MENG Zhaoqing;RONG Rong(School of Pharmacy,Shandong University of Traditional Chinese Medicine,Jinan 250355,China;Shandong Traditional Chinese Medicine Treatment of Respiratory Disease Technology Innovation Center Platform,Jinan 250103,China;Shandong Hongjitang Pharmaceutical Group Co.Ltd.,Jinan 250103,China)

机构地区：[1]山东中医药大学药学院,济南250355 [2]山东省中医药治疗呼吸系统疾病技术创新中心,济南250103 [3]山东宏济堂制药集团股份有限公司,济南250103

出　　处：《西南大学学报（自然科学版）》2023年第9期171-180,共10页Journal of Southwest University(Natural Science Edition)

基　　金：山东省重点研发计划(重大科技创新工程)项目(2020CXGC010505).

摘　　要：为了建立六金颗粒的制备方法及质量标准,中试规模制备六金颗粒,对制剂的成型性、吸湿性、溶化性、堆密度及流动性进行检测;采用薄层色谱法(TLC)对六金颗粒中锦灯笼进行定性鉴别;采用高效液相色谱法(HPLC)建立菊苣酸含量测定方法并进行方法学考察;采用HPLC法建立六金颗粒特征图谱,并进行峰归属及峰指认.结果发现,六金颗粒成型率达到98.1%,相关检查均符合规定;锦灯笼薄层色谱可检出特征斑点且阴性无干扰;菊苣酸含量方法学考察结果均符合要求,菊苣酸在1.44~86.19μg/mL范围内线性关系良好;通过不同条件的因素考察,确定了六金颗粒HPLC特征图谱色谱条件,方法学考察结果均符合要求,特征图谱中共确定8个特征峰,并指认了4个成分,分别为新绿原酸、单咖啡酰酒石酸、绿原酸和隐绿原酸.总之,六金颗粒制备工艺合理,建立的检测方法操作简单、重复性好,可为六金颗粒的质量评价和控制提供依据.To establish the preparation method and quality standard of Liujin granules,the formability,hygroscopicity,solubility,bulk density and fluidity of Liujin granules were determined.Thin layer chromatography(TLC)was used for qualitative identification of Physalis Calyx seu Fructus in the Liujin granules.High-performance liquid chromatography(HPLC)was used to establish a method for the determination of chicoric acid content.HPLC method was used to establish the characteristic spectrum of Liujin granules,and the peak attribution and identification were carried out.The molding ratio of compound Liujin granules was 98.1%,and the relevant inspections of the granules were in compliance with the regulations.The characteristic spots of Physalis Calyx seu Fructus could be detected by thin layer chromatography,and negative without interference.The results of the methodology for detection of chicoric acid content met the requirement.The linear relationship of chicoric acid was good in the range of 1.44~86.19μg/mL.The HPLC method for fingerprint analysis of Liujin granules were determined by examining the factors of different conditions.The results of methodological investigation are all in line with the requirements.Eight characteristic peaks were determined by the chromatographic characteristics,and 4 components were identified,namely neochlorogenic acid,moncafeoyl tartaric acid,chlorogenic acid and cryptochlorogenic acid.The preparation technology of Liujin granules is reasonable,the established detection method is simple and repeatable,which can provide reference for quality evaluation and control of Liujin granules.

关 键 词：六金颗粒 制备工艺 薄层色谱法 高效液相色谱法 特征图谱 

分 类 号：TQ460.6[化学工程—制药化工]