桔贝合剂质量标准提升研究  

Study on the improvement of quality standard for Jubei mixture

作　　者：洪挺 周志强 肖小武 陈丹丹 杨毅生 HONG Ting;ZHOU Zhiqiang;XIAO Xiaowu;CHEN Dandan;YANG Yisheng(Jiangxi Provincial Institute for Drug Control/NMPA Key Laboratory for Quality Evaluation of Chinese Patent Medicine/Jiangxi Provincial Engineering Research Center for Drug and Medical Device Quality,Nanchang 330029,China;College of Pharmacy,Jiangxi University of Chinese Medicine,Nanchang 330004,China)

机构地区：[1]江西省药品检验检测研究院/国家药品监督管理局中成药质量评价重点实验室/江西省药品与医疗器械质量工程技术研究中心,南昌330029 [2]江西中医药大学药学院,南昌330004

出　　处：《中国药房》2022年第21期2603-2608,共6页China Pharmacy

基　　金：国家药品标准制修订研究课题(No.2021Z026);江西省药品监督管理局科研项目(No.2019JS18)。

摘　　要：目的提升桔贝合剂的质量标准。方法采用三硝基苯酚与氢氰酸的化学反应鉴别苦杏仁水;采用薄层色谱(TLC)法定性鉴别桔贝合剂中桔梗、浙贝母、黄芩、枇杷叶、甘草;采用高效液相色谱(HPLC)法同时测定该制剂中苦杏仁苷、黄芩苷、汉黄芩苷、甘草酸铵4种成分的含量。结果三硝基苯酚试纸显砖红色。5味药材的TLC斑点清晰,阴性对照无干扰。苦杏仁苷、黄芩苷、汉黄芩苷和甘草酸铵的进样量线性范围分别为0.0668~1.3355μg(R^(2)=0.9994)、0.1898~3.7969μg(R^(2)=0.9999)、0.0626~1.2513μg(R^(2)=0.9999)、0.0418~0.8355μg(R^(2)=0.9998);精密度、重复性、稳定性试验的RSD均小于2%;平均加样回收率分别为98.2%、99.5%、98.3%、99.6%,RSD分别为0.7%,1.6%、1.5%、1.1%(n=6)。15批样品的含量存在差异,A公司样品的含量普遍低于B、C公司。结论所建质量标准可较好地反映桔贝合剂的内在质量。OBJECTIVE To improve the quality standard for Jubei mixture.METHODS The chemical reaction of trinitrophenol and hydrocyanic acid was used to identify Armeniacae Amarum solution.Platycodon grandiflorus,Fritillaria thunbergii,Scutellaria baicalensis,the leaves of Eriobotrya japonica and Glycyrrhiza uralensis in Jubei mixture were identified by thin-layer chromatography(TLC).High-performance liquid chromatography was used to simultaneously determine the contents of four active components,such as amygdalin,baicalin,wogonoside and monoammonium glycyrrhizinate in Jubei mixture.RESULTS Trinitrophenol test paper showed brick red.TLC spots of five medicinal materials were clear,without interference from negative control.The linear ranges of amygdalin,baicalin,wogonoside and monoammonium glycyrrhizinate were 0.0668-1.3355μg(R^(2)=0.9994),0.1898-3.7969μg(R^(2)=0.9999),0.0626-1.2513μg(R^(2)=0.9999),0.0418-0.8355μg(R^(2)=0.9998),respectively.RSDs of precision,repeatability and stability tests were all lower than 2%.The average recoveries were 98.2%,99.5%,98.3%,99.6%,and RSDs were 0.7%,1.6%,1.5%,1.1%(n=6).The contents of 15 batches of samples were different,and the content of sample from company A was generally lower than those from companies B and C.CONCLUSIONS The standard established can reflect the inherent quality of Jubei mixture well.

关 键 词：桔贝合剂 质量标准 化学反应 薄层色谱法 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学] R283.6[医药卫生—药学]