摘要
【目的】分离制备高纯度腺苷单体成分并研制国家标准样品。【方法】采取大孔树脂色谱、凝胶柱色谱与制备液相色谱相结合,建立了从瓜蒌皮中大量分离制备高纯度腺苷单体成分的方法,通过UV、IR、MS和NMR等技术进行结构鉴定及确证,按照ISO Guide 35和GB/T 15000.3-2008规程,对腺苷进行了均匀性、稳定性检验并通过8家实验室协作联合定值。【结果】获得标准值为99.89%、置信度95%下不确定度为0.18%的腺苷国家标准样品,均匀性符合标准,2~8℃条件下24个月内的长期稳定性良好,已获得专家组验收。【结论】该高纯度腺苷制备方法具有制备成本低、操作简便、效率高的特点,解决了腺苷国家标准样品缺乏的问题,为我国瓜蒌药材及相关制品的生产质量控制及分析检测提供了物质基础。
【Objective】The study was conducted to separate and prepare high-purity adenosine component and develop a certified reference material(CRM)of adenosine.【Method】A method was established to separate and prepare a large amount of high-purity adenosine from Trichosanthes kirilowii Maxim.fruit peel by macroporous resin chromatography combined with gel column chromatography,preparative liquid chromatography.The structure of adenosine was identified and confirmed by means of UV,IR,MS and NMR.The homogeneity and stability of adenosine samples were tested and passed the certification jointly conducted by 8 laboratories according to the technical requirements of ISO Guide 35 and GB/T 15000.3-2008.【Result】The standard value was determined to be 99.89%and the uncertainty of confidence-level of 95%was 0.18%.The uniformity of prepared samples well met the standard,and they were stable for 24 months under the storage condition of 2-8℃,and accepted by the expert group.【Conclusion】The preparation method of high-purity adenosine has the characteristics of low preparation cost,simple operation and high efficiency,which solves the problem of the lack of national standard samples for adenosine,and provides material basis to quality control,analysis and testing of T.kirilowii Maxim.medicinal materials and related products in China.
作者
李兆
李景超
王岱杰
赵恒强
刘伟
崔莉
LI Zhao;LI Jingchao;WANG Daijie;ZHAO Hengqiang;LIU Wei;CUI Li(Qilu University of Technology(Shandong Academy of Sciences),Shandong Analysis and Test Center/Shandong Key Laboratory for Applied Technology of Sophisticated Analytical Instruments,Jinan 250014,China)
出处
《广东农业科学》
CAS
2021年第2期146-152,共7页
Guangdong Agricultural Sciences
基金
山东省重点研发计划项目(2019GSF108035,2017CXGC1304)
济南市农业应用技术创新计划项目(201913)。
关键词
腺苷
分离制备
标准样品
稳定性
adenosine
separation and preparation
certified reference material
stability
