摘要
依据GB/T 15000.3-2008《标准样品工作导则(3)标准样品定值的一般原则和统计方法》,研制熊果酸标样样品。以蔷薇科植物山楂Crataegus pinnatifida Bge.的干燥成熟果实为原料,采用大孔树脂富集,硅胶柱色谱分离结合重结晶的方法制备熊果酸单体,通过紫外光谱、红外光谱、质谱和核磁共振等手段进行结构表征,同时进行薄层色谱鉴别和热重分析,建立高效液相色谱(high performance liquid chromatography,HPLC)检测分析技术。熊果酸样品进行均匀性检验、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24个月稳定性良好,定值结果确定其标准值为99.80%,置信度95%的不确定度为0.18%。成功研制出了熊果酸国家标准样品,达到了GB/T 15000.3-2008规定的技术要求,样品具有溯源性,可用于熊果酸及相关产品的质量控制和检测方法评定。
To developing a certified reference material(CRM)of ursolic acid according to the technical requirements of GB/T 15000.3-2008<CRM General and Statistical Principle for Certification>.Ursolic acid samples were obtained by means of macroporous resin,silica gel chromatography,and recrystallization from dried fruit of Crataegus pinnatifida Bge.,and their structures were confirmed by ultraviolet spectrum,infrared spectrum,mass spectrum and nuclear magnetic resonance spectrum.Ursolic acid samples were analyzed by thin layer chromatography,thermo-gravimetric and high performance liquid chromatography(HPLC)analysis technology.The ursolic acid samples were divided into bottles for homogeneity test,stability test,and cooperative certification by eight laboratories.The results showed that the homogeneity of ursolic acid samples were excellent,with good stability within 24 months at 0-4℃.The certified value of the reference material of ursolic acid was 99.80%with the expanded uncertainty of 0.18%in confidence coefficient of 95%.The reference material of ursolic acid was successfully developed.It was conformed to the technical requirement of GB/T 15000.3-2008 and could be traceable.The CRM can be used in the content determination and testing method validation of ursolic acid related products.
作者
王岱杰
于金倩
崔莉
付瑞明
宋祥云
耿岩玲
WANG Dai-jie;YU Jin-qian;CUI Li;FU Rui-ming;SONG Xiang-yun;GENG Yan-ling(Shandong Analysis and Test Center,Key Laboratory of TCM Quality Control,Jinan 250014,Shandong,China)
出处
《食品研究与开发》
CAS
北大核心
2018年第22期79-85,共7页
Food Research and Development
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
山东省科学院先导支持项目
关键词
熊果酸
标准样品
均匀性
稳定性
定值
不确定度
ursolic acid
certified reference material
homogeneity
stability
certification
uncertainty
