海藻糖标准样品的研制  

Development of Trehalose Certified Reference Material

作　　者：陈晖[1,2] 方华[1] 张怡评[1] 陈伟珠[1] 洪专[1] 易瑞灶[1] 

机构地区：[1]国家海洋局第三海洋研究所,福建厦门361005 [2]厦门大学海洋与地球学院,近海海洋环境科学国家重点实验室,福建厦门361005

出　　处：《化学分析计量》2015年第1期1-4,共4页Chemical Analysis And Meterage

基　　金：福建省科技计划项目(2013N01010205);厦门市海洋经济创新发展区域示范项目(12PZP001SF10);海洋公益行业科研专项(201005020–1);厦门市科技计划项目(3502Z20122009)

摘　　要：研制了海藻糖国家标准样品。以食品级海藻糖粗品为原料,纯化制备海藻糖,采用红外光谱(IR)、质谱和核磁共振谱(NMR)以及单晶衍射等方法进行结构确证。样品分装成400瓶后,采用离子色谱法进行均匀性、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%的置信区间范围内,样品均匀性良好。在40℃下,经过24个月稳定性考察,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,并评定了定值结果的不确定度,海藻糖标准样品定值结果为99.72%,扩展不确定度为0.26%(k=1.96)。该标准样品达到国家标准样品的技术要求,可用于有关海藻糖的方法校正和质量控制。Trehalose certified reference material was developed.Trehalose was purified from the crude product.The structure of trehalose certified reference material was comfirmed by infrared spectroscopy （IR）,mass spectrometry,NRM and XRD.Trehalose was divided into 400 bottles.The homogeneity and stability testing and quantitative analysiswere evaluated by ion chromatography method.According to analysis procedure of homogeneity,15 bottles of samplewere randomly taken from 400 bottles,and the results were validated by F-test statistical methods.The stability inspectionwas carried on the long-term（24 months）,and the results indicated that the period for trehalose storage was 24months at 40℃ .A cooperative certification was conducted by 8 qualified laboratories.The certified purity value of thereference material of trehalose was 99.72%with relative expaned uncertainty of 0.26%（k=1.96）.The reference materialcan conform to the technical requirement of the certified reference material,and it can be used for validation and qualitycontrol regarding trehalose.

关 键 词：海藻糖 标准样品 离子色谱法 定值 不确定度 

分 类 号：O653[理学—分析化学]