橙皮素标准样品的研制  

Preparation of certified reference materials of hesperetin

作　　者：宋祥云[1] 刘金宇 耿岩玲[1] 林云良[1] 付瑞明 崔莉[1] 王岱杰[1] 

机构地区：[1]山东省分析测试中心,山东省中药质量控制技术重点实验室,山东济南250014 [2]鲁南制药集团股份有限公司,山东临沂276006

出　　处：《山东科学》2018年第1期16-22,共7页Shandong Science

基　　金：山东省重大科技创新工程(2017CXGC1308);山东省重点研发计划(2017GSF216002)

摘　　要：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.

关 键 词：橙皮素 标准样品 均匀性 稳定性 定值 不确定度 

分 类 号：R284.2[医药卫生—中药学]