橙皮素标准样品的研制

Preparation of certified reference materials of hesperetin

建立了橙皮素标准样品的研制方法。采用硅胶柱色谱结合制备液相色谱技术对橙皮素样品进行分离制备,通过UV、IR、MS和NMR等手段进行结构表征,同时进行了薄层色谱鉴别和热重分析,进行了均匀性、稳定性检验和8家实验室联合定值。结果表明,该样品均匀性良好,在0~4℃储存条件下12个月稳定性良好,定值结果确定其标准值为98.78%,置信度95%的不确定度为0.26%。该橙皮素标准样品达到了国家标准样品的技术要求,具有溯源性,可用于橙皮素及相关产品的质量控制和检测方法评定。

A method for the preparation of the certified reference material （CRM） of hesperetin was established in this article. Hesperetin sample was obtained by means of silica gel chromatography combined with preparative HPLC technique, and its structure was characterized by UV, IR, MS and NMR. At the same time, the TLC identification and thermo-gravimetric analysis were carried out, and the sample was divided into bottles for further homogeneity test, stability test, and the cooperative certification by 8 laboratories. The results indicated that hesperetin samples had good homogeneity, with good stability within ]2 months at 0-4 %. The certified value of the reference material of hesperetin was 98.78%, with the expanded uncertainty of 0.26% in confidence coefficient of 95%. The standard sample of hesperetin has reached the technical requirements of the national certified reference material. The CRM has traceability and can be used in the content determination, testing method validation, as well as t quality control of hesperetin and related products.