樱花素标准样品的研制

Preparation of Certified Reference Material of Sakuranetin

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,研制樱花素国家标准样品。方法:以中药毛白杨的干燥茎皮为原料,通过提取、分离,纯化制备了樱花素样品,采用旋光度、元素分析、红外光谱、紫外光谱、高分辨质谱、核磁共振谱和X-单晶衍射进行了结构鉴定。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400瓶(每瓶5 mg)后,进行了均匀性检验、稳定性检验和联合定值。结果:该样品为DL-5,4'-二羟基-7-甲氧基二氢黄酮,95%置信区间范围内的均匀性良好,0~8℃条件下24个月内稳定性良好,定值结果确定其纯度为99.97%,相对扩展不确定度为0.02%,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:成功地研制了樱花素国家标准样品,可用于樱花素含量测定、检测方法评定、相关产品的检测与质量控制。

Objective： To develop a certified reference material（ CRM） of sakuranetin according to the Work Guideline for Reference Materials（ 3） ： Reference Material-General Principles and Statistical Method for Certification（ GB / T 15000. 3-2008） upon the approved by Standardization Administration of China（ SAC）.Method： Sakuranetin was extracted from dried barks of Populus tomentosa. The structure of sakuranetin was identified by optical rotation,elemental analysis,IR,UV,high-resolution MS,NMR,and X-ray diffraction analysis. Thin layer chromatography was carried out for the identification. Sakuranetin was divided into 400 bottles,with 5 mg per bottle. The homogeneity test,stability test,and quantitative analysis were carried out by highperformance liquid chromatography-ultra violet detector. Result： This CRM is DL-5, 4＇-dihydroxy-7-methoxyflavanone. The homogeneity of the 95% confidence interval was good. The storage period was 24 months at0-8 ℃. The certified purity value was 99. 97%,with a relative expanded uncertainty of 0. 02%. The CRM of sakuranetin reached the technical requirements of CRM,and was accepted by SAC. Conclusion： The CRM of sakuranetin is successfully developed,and can be used for determining content,evaluating test methods,detecting relevant products and controlling quality.