不同国家药典对甘草酸单铵盐有关物质及含量测定结果与建立方法的比较  

Comparison of Quantitative Determination of Principal Component Isomer and Related Substances of Ammonium Glycyrrhizinate by Component and Related Substances of Ammonium Glycyrrhizinate by Methods Contained in Different Pharmacopoeias and a New Method Esta

作　　者：赵燕燕[1,2] 刘丽艳[1] 韩媛媛[1] 李月秋[1] 王艳[3] 石敏健[3] 

机构地区：[1]河北大学医学实验中心,河北保定071000 [2]河北大学化学与环境科学学院河北省分析科学技术重点实验室河北省化学生物学重点实验室,河北保定071002 [3]河北大学化学与环境科学学院,河北省分析科学技术重点实验室河北省化学生物学重点实验室,河北保定071002

出　　处：《中国药学杂志》2013年第22期1944-1950,共7页Chinese Pharmaceutical Journal

基　　金：河北省自然基金资助项目(H2013201203);河北教育厅科学研究计划资助项目(2009315);河北省卫生厅医学科学研究重点课题计划资助项目(20090570);河北省中医药管理局科研计划资助课题(2008072)

摘　　要：目的通过分析不同国家药典或药品标准以及本实验建立的对甘草酸单铵盐主成分及其有关物质的检测方法,对含量测定结果进行比较,以对检测方法进行评价。方法采用欧洲、英国最新版药典以及中国国家药品标准所收载的甘草酸单铵盐质量标准中的方法和本实验建立的方法,分别对其原料药和制剂中主成分及有关物质进行测定,对其色谱行为、主成分异构体分离度、实验成本、方法学、含量测定结果以及各方法的优缺点等进行比较和研究,并给出综合评价。结果现有各国药典或药品标准所用流动相均为酸性体系,对主成分异构体18α-Gly、18β-Gly没有分离选择性,不能真实反映原料药和制剂中18α-Gly、18β-Gly、有关物质A和有关物质B的含量;本实验建立的方法对主成分异构体的分离度为1.5,符合药典要求。欧洲药典EP 7.0版、英国药典2012版和中国国家药品标准(WS1-XG-2002)收载的甘草酸单铵盐质量标准中的含量测定方法与本实验建立的方法比较,对样品中主成分及有关物质的含量测定结果无显著性差异。结论综合准确性、实用性等方面因素,本实验建立的方法,能够实现对主成分异构体的有效分离;分析检测成本、毒性和污染均降低,分析检测时间缩短,检出限降低,结果准确、可靠;为甘草酸单铵盐类原料药和制剂内在质量控制、为将来各国对药典收载的甘草酸单铵盐质量标准的增补与修订提供依据。To determine and compare the contents of principal component and related substances of ammonium glycyrrhizinate by methods contained in different pharmacopoeias and a new method established by our lab. METHODS The methods for quality control of ammonium glycyrrhizinate in the latest edition of European Pharmacopoeia, British Pharmacopoeia, national drug standards of China, and the method established by our laboratory were employed to determine the contents of the principal component isomers and related substances of ammonium glycyrrhizinate in its raw materials and pharmaceutical products. The methods were evaluated and compared regarding the chromatographic features, resolution of principal component isomers, experimental cost, content determination results, and the advantages and disadvantages of each method were discussed. RESULTS The mobile phases adopted in aforementioned pharmacopoeias are all acidic, which could not effectively separate 18α-glycyrrhizinic acid and 18β-glycyrrhizinic acid, thus could not truly reflect the contents of 18α-glycyrrhizinic acid, 18β-glycyrrhizinic acid, related substances A, and the related substances in the raw materials and pharmaceutical products. The resolution of principal component isomer by our method was 1.5, complying to the pharmacopoeia requirement. The content determination results of ammonium glycyrrhizinate raw materials by the four methods had no significant difference. CONCLUSION Among the four methods, the method established by our laboratory performed best in terms of accuracy and practicability. This method has shorter detection time, lower cost, reduced toxicity and pollution, and the results are accurate and reliable, which suggests that it can be used for the chiral resolution of 18α-glycyrrhizinic acid and 18β-glycyrrhizinic acid and the content determination of principal component and related substances of the raw material and pharmaceutical products of ammonium glycyrrhizinate. This study provideds reference for further revision of the quality con

关 键 词：药典 甘草酸单铵盐 原料药 制剂 有关物质 含量检测 

分 类 号：R917[医药卫生—药物分析学]