芝麻素标准样品的研制

Preparation of certified reference material of sesamin

依据GB/T 15000.3—2008《标准样品工作导则》,研制芝麻素标准样品。以芝麻为原料,采用高速逆流色谱法分离制备芝麻素单体,通过UV、IR、MS和NMR等手段进行结构表征,同时进行薄层色谱鉴别和热重分析。芝麻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℃条件下储存36个月稳定性良好,定值结果确定其标准值为99.73%,置信度95%的不确定度为0.20。成功研制出了芝麻素国家标准样品,达到了GB/T 15000.3—2008规定的技术要求,样品具有溯源性,可用于芝麻素及相关产品的质量控制和检测方法评定。

A certified reference material （CRM） of sesamin was developed according to the technical requirements of CRM General and Statistical Principle for Certification （ GB/T 15000.3-2008 ）. Sesamin monomer was prepared from sesame by means of high - speed counter - current chromatography, and its structure was confirmed by UV, IR, MS and NMR. Sesamin sample was analyzed by thin layer chroma- tography and thermo - gravimetric analysis. Also it was tested for homogeneity test, stability test, and cooperative certification by eight laboratories. The results indicated that the homogeneity of sesamin was excellent, with good stability within 36 months at 0 - 4 ℃. The certified value of the reference material of sesamin was 99.73 % with the expanded uncertainty of 0.20 in confidence coefficient of 95 %. The certi- fied reference material of sesamin was successfully developed. It was conformed to the technical require- ment of GB/T 15000.3--2008 and could be traceable. The CRM could be used in the content determina- tion and testing method validation of sesamin related products.