摘要
目的: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》,在国家标准化管理委员会批准立项的基础上,研制长梗冬青苷标准样品。方法:以冬青科植物铁冬青的干燥树皮为原料,通过大孔树脂吸附技术和高速逆流色谱技术,纯化和制备了长梗冬青苷样品,采用元素分析、紫外光谱、红外光谱、高分辨质谱、核磁共振谱和X-单晶衍射进行了结构确定,进行了薄层色谱的鉴别,建立了高效液相色谱紫外检测分析技术。样品分装成600瓶,每瓶5 mg,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:该样品在95%的置信区间范围内均匀性良好,在0~8℃条件下24个月内稳定性良好,定值结果确定其纯度为99.60%,扩展不确定度为0.10%,通过了国家标准化管理委员会组织的验收,达到了国家标准样品的技术要求。结论:成功地研制了长梗冬青苷国家标准样品,纯度高于市售对照品,可用于长梗冬青苷的含量测定、检测方法评定和相关产品的检测与质量控制。
Objective： To develop a certified reference material （CRM） of pedunculoside according to the Directives for CRM General and Statistical Principle for Certification （GB/T 15000.3-2008 ） based on the CRM project approved by Standardization Administration of the People＇s Republic of China （SAC）. Method： Pedunculoside samples were obtained by means of macroporous resin enrichment, high speed counter-current chromatography, and recrystalization from the dried bark of llex rotunda, and their structures were confirmed by element analysis, UV, IR, HR-MS, NMR, and XRD. In addition, thin layer chromatography was carried out for identification, and high performance liquid chromatography ultraviolet detection and analysis technology was established. The pedunculoside samples divided into 600 bottles with 5 mg per bottle for homogeneity test, stability test, and cooperative certification by 8 laboratories. Result： The homogeneity of pedunculoside samples was excellent in 95 % confidence interval, with good stability within 24 months at 0-8 ℃. The certified purity value of the pedunculoside samples was 99.60% with an expanded uncertainty of 0. 10% （k = 2.00）. They were approved by the National Standardization Management Committee, and consistent with the technical requirements of the national standard samples. Conclusion： National certified reference materials for pedunculoside were successfully studied and developed for the first time, and their purity was higher than that of samples purchased from markets, so this method can be used in the content determination, testing method validation, as well as testing and quality control of pedunculoside products.
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2017年第12期65-70,共6页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家质量监督检验检疫总局行业科研专项(201210209)
国家标准化管理委员会国家标准样品研制项目(S2012087)
关键词
长梗冬青苷
标准样品
均匀性
稳定性
定值
不确定度
pedunculoside
certified reference material
homogeneity
certification
uncertainty stability
作者简介
马玉翠，在读硕士，从事天然产物国家标准样品的研制，Tel：1590126328，E-mail：872018483@qq.com
[通讯作者]巢志茂，研究员，博士生导师，从事天然产物国家标准样品的研制，Tel：13522705161，E-mail：chaozhimao@163.com
