章鱼肉碱标准样品的研制  

Development of Octopine Certified Reference Material

作　　者：谢全灵[1] 张怡评[1] 陈晖[1] 洪专[1] 陈伟珠[1] 方华[1] 

机构地区：[1]国家海洋局第三海洋研究所福建省海洋生物资源开发利用协同创新中心,福建厦门361005

出　　处：《化学分析计量》2016年第3期4-7,29,共5页Chemical Analysis And Meterage

基　　金：厦门市科技计划项目(NO.3502Z20130004);海洋公益性行业科研专项(201205022–8);广东海洋经济发展区域示范项目(GD2012–D01–001)

摘　　要：研制了章鱼肉碱标准样品.以章鱼加工副产物为原料,通过提取、分离纯化制备高纯章鱼肉碱,采用红外光谱（IR）、高分辨质谱（MS） 和核磁共振谱（NMR） 进行结构确证.样品分装成144 瓶,采用离子色谱检测法进行均匀性、稳定性检验和定值分析.从样品中随机抽取15 瓶进行均匀性检验,经F 检验表明在95% 的置信区间内样品均匀性良好.在0～4℃条件下,经过24 个月长期试验稳定性考察,结果表明样品稳定性良好.标准样品经国内8 家具有分析资质的实验室进行协同定值,章鱼肉碱标准样品定值结果为99.49%,相对扩展不确定度为0.14%（k=1.96）.该标准样品达到标准样品的技术要求,可用于章鱼肉碱相关产品的质量控制和分析方法校正.Octopine certified reference material was developed. Octopine was made from the processing byproduct of octopus. The structure of octopine certified reference material was comfirmed by infrared spectroscopy(IR),high resolution mass spectral(HRMS) and nuclear magnetic resonance(NMR). Octopine was divided into 144 bottles. The homogeneity and stability testing and quantitative analysis method were evaluated by ions chromatography. According to analysis procedure of homogeneity,15 bottles of sample were randomly taken from 144 bottles,the sample homogeneity of inspection validated by F–test statistical methods within the 95% confidence interval was good. The stability inspection was carried on the long-term(24 months),and the results indicated that the period for octopine of storage was 24 months at 0 – 4℃. A cooperative certification was conducted with 8 qualified laboratories. The certified purity value of the reference material of octopine was 99.49% with the relative expaned uncertainty of 0.14 %(k=1.96). The reference material can conform to the technical requirement of the certified reference material. The material was intended for use in the method validation and quality control regarding octopine.

关 键 词：章鱼肉碱标准样品 均匀性 稳定性 定值 不确定度 

分 类 号：O656[理学—分析化学]