白果内酯标准样品的研制  

Preparation of certified reference material of bilobalide

作　　者：付瑞明 胡金春 孟兆青 李强[1] 曹桂云 王岱杰 闫慧娇 FU Rui-ming;HU Jin-chun;MENG Zhao-qing;LI Qiang;CAO Gui-yun;WANG Dai-jie;YAN Hui-jiao(Shandong Provincial Key Laboratory of Applied Technology of Sophisticated Analytical Instruments,Shandong Analysis and Test Center,Qilu University of Technology(Shandong Academy of Sciences),Jinan 250014,China;Shandong Hongjitang Pharmaceutical Group Co.,Ltd.,Jinan 250103,China)

机构地区：[1]齐鲁工业大学(山东省科学院)山东省分析测试中心山东省大型精密仪器分析应用技术重点实验室,山东济南250014 [2]山东宏济堂制药集团股份有限公司,山东济南250000

出　　处：《山东科学》2022年第1期6-13,共8页Shandong Science

基　　金：泉城产业领军人才支持计划;齐鲁工业大学(山东省科学院)科教产融合创新试点工程(2020KJC-GH08)。

摘　　要：建立了银杏叶中白果内酯标准样品的制备方法。以银杏的干燥叶为原料,采用硅胶柱色谱结合凝胶柱色谱富集和制备液相精制的方法,制备白果内酯单体,采用紫外光谱、红外光谱、质谱和核磁共振等技术进行结构确证与表征,按照GB/T 15000.3—2008/ISO Guide 35:2006的规程,进行了均匀性、稳定性检验和8家实验室协作联合定值。结果表明,制备的白果内酯国家标准样品纯度标准值为99.88%,置信度95%的不确定度为0.22%,均匀性符合标准,在2~8℃条件下贮藏24个月稳定性良好。该方法具有制备成本低、操作简便、效率高的特点,解决了白果内酯国家标准样品缺乏的问题,为白果内酯及相关产品的生产质量控制及分析检测提供了物质基础。A preparation method for bilobalide certified reference material(CRM)was developed in this study to enrich and prepare bilobalide from ginkgo biloba using silica gel column chromatography combined with gel column chromatography and preparative liquid chromatography.The structure of bilobalide was characterized using UV,IR,MS,and NMR.Bilobalide samples were tested for homogeneity and stability according to the technical requirements of GB/T 15000.3—2008/ISO Guide 35:2006.Cooperative certification was conducted by eight laboratories.The results indicated that the standard value was 99.88%and the uncertainty was 0.22%with a confidence interval of 95%.The prepared samples had good uniformity and were stable for 24 months at storage temperatures of 2~8°C,which were acceptable to the expert group.The preparation method of high-purity bilobalide has low preparation cost,simple operation,and high efficiency,which solves the problem of the lack of national standard samples for bilobalide and can be applied for quality control,analysis,and testing of Chinese medicinal materials and related products.

关 键 词：白果内酯 标准样品 均匀性 稳定性 定值 

分 类 号：R284.2[医药卫生—中药学]