异补骨脂素标准样品的研制  

Preparation of certified reference materials of isopsoralen

作　　者：林云良 耿岩玲 于金倩 朱姮 付瑞明 王岱杰 LIN Yun-liang;GENG Yan-ling;YU Jin-qian;ZHU Heng;FU Rui-ming;WANG Dai-jie(Qilu University of Technology（Shandong Academy of Sciences）,Shandong Analysis and Test Center,Key Laboratory of TCM Quality Control,Jinan 250014)

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中药质量控制技术重点实验室,济南250014

出　　处：《分析试验室》2018年第10期1165-1169,共5页Chinese Journal of Analysis Laboratory

基　　金：山东省重大科技创新工程(2017CXGC1209;2017CXGC1308);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资助

摘　　要：依据GB/T 15000.3-2008标准样品的工作导则,研制异补骨脂素标样样品。采用豆科植物补骨脂Psoralea corylifolia L.的干燥成熟果实为原料,高速逆流色谱法分离制备异补骨脂素单体,通过紫外光谱、红外光谱、质谱和核磁共振等技术进行结构表征,同时进行了薄层色谱鉴别和热重分析,建立了HPLC检测分析方法。异补骨脂素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。结果表明,该样品均匀性良好,在0~4℃储存条件下48个月稳定性良好,定值结果确定其标准值为99.83%,置信度95%的不确定度为0.22%。A certified reference material （CRM） of isopsoralen was prepared according to the technical requirements of CRM General and Statistical Principle for Certification （GB/T 15000. 3 -2008 ）. Isopsoralen samples were obtained by means of high-speed counter-current chromatography from dried fruit of Psoralea corylifolia L., and their structures were confirmed by UV, IR, MS and NMR. Isopsoralen samples were analyzed by thin layer chromatography, thermo-gravimetric and HPLC analysis technology. The isopsoralen samples were divided into bottles for homogeneity test, stability test, and cooperative certification by eight laboratories. The results indicated that the homogeneity of isopsoralen samples were excellent, with good stability within 48 months at 0 -4℃. The certified value of the reference material of isopsoralen was 99.83% with the expanded uncertainty of 0. 22% in the confidence coefficient of 95%.

关 键 词：异补骨脂素 标准样品 均匀性 稳定性 定值 不确定度 

分 类 号：R917[医药卫生—药物分析学]