蔗果三糖标准样品的研制

Preparation of Kestose Certified Reference Materials

根据GB/T15000-2008《标准样品工作导则》的要求,建立蔗果三糖标准样品的研制方法。采用P-2凝胶色谱法结合制备高效液相色谱法从低聚果糖产品中制备得到蔗果三糖,然后通过红外光谱、质谱、核磁共振谱(1HNMR、13CNMR、HMBC、NMQC、COSY)对样品的结构进行鉴定并对核磁信号进行归属。将样品分装成130瓶后,采用高效液相-蒸发光散射法进行均匀性和稳定性检验,通过对8家具有资质的实验室联合测定结果的数据分析,评定出定值结果和不确定度。结果表明:蔗果三糖标准样品的稳定性和均匀性良好,定值结果为99.87%,置信度为95%的不确定度是0.36%。研制出的蔗果三糖标准样品符合国家标准样品研制工作导则的技术要求,可用于有关蔗果三糖和低聚果糖产品的检测和质量控制。

According to the directives for the work of reference materials GB/T15000-2008,a method was developed to prepare kestose certified reference material. Kestose was isolated by P-2 gel and pre-HPLC from fructooligosaccharide,and its structure was identified by IR,UV,LC-MS,and NMR（1HNMR,13 CNMR,HMBC,NMQC,COSY）. Kestose was divided into 130 aliquotes. The homogeneity and stability test were carried out by HPLC-ELSD. A cooperative certification was conducted with 8 laboratories and the certification data were analyzed.The results showed that the certified value of the reference material of kestose was 99.87 % with the expanded uncertainty of 0.36 % in confidence coefficient of 95 %. The reference material of kestose conformed to the directive for the work of reference materials,and can be used for correcting and quality control of related productes.