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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: Based on the general principles and statistical methods of GB / T 15000.3-2008 “Guidelines for Standard Sample Work (3) Standards” and the approval of the National Standardization Management Committee, saikosan national standard samples were developed. Methods: The saponins of Populus tomentosa were prepared by extraction, separation and purification using optical spectra, elemental analysis, IR, UV, 1H-NMR and X-ray crystal Diffraction was identified by structure. TLC was identified. The establishment of a high performance liquid chromatography UV detection and analysis technology. After the samples were dispensed into 400 bottles (5 mg per bottle), homogeneity tests, stability tests, and combined settings were performed. Results: The sample was DL-5,4’-dihydroxy-7-methoxy-flavanone with a good 95% confidence interval, good stability within 24 months at 0-8 ℃, The value of the results to determine the purity of 99.97%, the relative expansion of the uncertainty of 0.02%, passed the inspection and acceptance of the National Standardization Management Committee, has reached the national standard samples of the technical requirements. Conclusion: The saikosaponin national standard sample has been successfully developed and can be used for the determination of sakuraidin, the assessment of test methods, the detection and quality control of related products.