水苏糖标准样品的研制

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。

Development of Certified Reference Material of Stachyose

Objective: To develop a certified reference material (CRM) of stachyose according to Directives for the Work of CRM (3) Reference Materials: General and Statistical Principle for Certification (GB/T 15000.3-2008). Method: Stachyose was prepared by extraction, fermentation, separation and purification with the dried rhizome of Stachys floridana as the raw materials. The structure of stachyose was confirmed by element analysis, UV, IR, HR-MS, NMR and X-single crystal diffraction. The samples of stachyose were divided into 400 bottles with 10 mg/bottle. Then the homogeneity test, stability test and quantitative analysis were carried out by high performance liquid chromatography-evaporative light-scattering detector. Result: The samples showed good homogeneity at 95% confidence interval and good stability within 24 months; the certified purity value was 99.62% with an expanded uncertainty of 0.13%. The samples were checked and accepted by Standardization Administration of China, and were consistent with the technical requirement of a series of GB/T 15000.3 guides about CRM. Conclusion: The national CRM of stachyose was developed for the first time, and this CRM was intended for use in the content determination, method validation as well as testing and quality control of stachyose.