白鲜碱标准样品的研制  

Preparation of certified reference materials of dictamnine

作　　者：耿岩玲[1] 宋祥云[1] 王晓[1] 林云良[1] 朱姮 王岱杰[1] GENG Yan-ling;SONG Xiang-yun;WANG Xiao;LIN Yun-liang;ZHU Heng;WANG Dai-jie(Shandong Analysis and Test Center,Key Laboratory of Traditioal Chinese Medicine Quality Control,Ji＇nan 250014,China)

机构地区：[1]山东省分析测试中心山东省中药质量控制技术重点实验室,山东济南250014

出　　处：《时珍国医国药》2018年第7期1603-1606,共4页Lishizhen Medicine and Materia Medica Research

基　　金：山东省重大科技创新工程(2017CXGC1308;2017CXGC1209);山东省重点研发计划(2017GSF216002);山东省泰山学者岗位专家支持项目;山东省科学院先导项目

摘　　要：目的依据GB/T 15000.3-2008标准样品的工作导则,研制白鲜碱标样样品。方法以芸香科植物白鲜Dictamnus dasycarpus Turcz的干燥根皮为原料,采用硅胶柱色谱结合高速逆流色谱分离制备白鲜碱单体,通过UV、IR、MS和NMR等手段进行结构表征,同时进行了薄层色谱鉴别和热重分析,建立了HPLC检测分析技术。白鲜碱样品进行了均匀性检验、稳定性检验和8家实验室联合定值。结果结果制备的样品均匀性良好,在0~4℃储存条件下24个月稳定性良好,定值结果确定其标准值为99.85%,置信度95%的不确定度为0.24%。结论成功研制出了白鲜碱国家标准样品,达到了GB/T 15000.3-2008规定的技术要求,样品具有溯源性,可用于白鲜碱及相关产品的质量控制和检测方法评定。Objective To develop a certified reference material（ CRM） of dictamnine according to the technical requirements of CRM General and Statistical Principle for Certification（ GB/T 15000. 3-2008）. Methods Dictamnine samples were obtained by means of silica gel high-speed counter-current chromatography from dried bark of Dictamnus dasycarpus Turcz,and their structures were confirmed by UV,IR,MS and NMR. Dictamnine samples were analyzed by thin layer chromatography,thermo-gravimetric and HPLC analysis technology. The dictamnine samples were divided into bottles for homogeneity test,stability test,and cooperative certification by 8 laboratories. The results indicated that the homogeneity of dictamnine samples were excellent,with good stability within 24 months at 0-4℃. The certified value of the reference material of dictamnine was 99. 85% with the expanded uncertainty of 0. 24% in confidence coefficient of 95%. Results The reference material of dictamnine was successfully developed It was conformed to the technical requirement of GB/T 15000. 3-2008 and could be traceable. Conclusion The CRM can be used in the content determination and testing method validation of dictamnine related products.

关 键 词：白鲜碱 标准样品 均匀性 稳定性 定值 不确定度 

分 类 号：R284.2[医药卫生—中药学]