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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》,研制水苏糖标准样品。方法:以唇形科植物银条Stachys floridana新鲜的地下茎为原料,通过提取、发酵、分离、纯化制备水苏糖。采用元素分析,UV,IR,HR-MS,NMR和X-单晶衍射进行结构鉴定。样品分装成400瓶(每瓶10 mg)后,采用高效液相色谱法-蒸发光散射检测器进行均匀性、稳定性检验和定值分析。结果:该标准样品95%置信区间范围内均匀性良好,24个月内稳定性良好,定值结果确定纯度为99.62%,扩展不确定度为0.13%,通过了国家标准化管理委员会组织的验收,达到了GB/T 15000.3系列国家标准样品的技术要求。结论:首次研制了水苏糖国家标准样品。本标准样品可用于水苏糖含量测定、检测方法评定、相关产品的检测与质量控制。
OBJECTIVE: To develop stachyose standard samples according to GB / T 15000.3-2008 Standard Guide for Standard Samples (3) Standard Samples: General Principles and Statistical Methods for Setting Values. Methods: Stachys floridana was used as raw material for the preparation of stachyose by extraction, fermentation, separation and purification. Structural analysis was carried out by elemental analysis, UV, IR, HR-MS, NMR and X-ray single crystal diffraction. After the sample was dispensed into 400 bottles (10 mg per bottle), HPLC, evaporative light scattering detector was used for homogeneity, stability test and value analysis. Results: The 95% Confidence Interval of the standard sample was well-homogenized within 24 months. The stability was good within 24 months. The purity of the standard sample was 99.62% and the uncertainty of expansion was 0.13%. It passed the acceptance test of the National Standardization Management Committee, Achieved GB / T 15000.3 series of national standards for the technical requirements of the sample. Conclusion: The stachyose national standard sample was developed for the first time. This standard sample can be used for the determination of stachyose content, testing methods, testing and quality control of related products.