液相色谱法测定乳粉中唾液酸含量的不确定度评定  

Uncertainty evaluation of the determination of sialic acid in milk powder by high performance liquid chromatography

作　　者：钱振杰 陈敬 游淑珠 赵悦 何咏欣 冯家望 QIAN Zhenjie;CHEN Jing;YOU Shuzhu;ZHAO Yue;HE Yongxin;FENG Jiawang(Guangzhou Institute for Food Inspection,Guangzhou 511400,China;Gongbei Customs Technology Center,Zhuhai 519000,China)

机构地区：[1]广州市食品检验所,广州511400 [2]拱北海关技术中心,广东珠海519000

出　　处：《化学分析计量》2022年第12期78-82,共5页Chemical Analysis And Meterage

基　　金：珠海市重点科技项目(ZH22036201210211PWC)。

摘　　要：评定液相色谱法测定乳粉中唾液酸含量的测量不确定度。用酸水解法释放乳粉中的唾液酸,再与邻苯二胺衍生,采用液相色谱分离,荧光检测器检测,外标法定量。分别考察每个测量步骤不确定度的来源,并对各个因素引入的不确定度进行计算与合成,得到测量结果的扩展不确定度。当乳粉中唾液酸含量为2 586 mg/kg时,扩展不确定度为153 mg/kg,包含因子k=2。造成唾液酸测定结果不确定度偏高的主要因素是标准工作液配制、样品定容及测量重复性误差三方面。在日常检验过程中应采用加强操作规范性、配制适合浓度范围的标准溶液、增加平行样品的测定次数等措施保证测量结果的科学性与准确性。The uncertainty in determination of sialic acid in milk powder by high performance liquid chromatography was evaluated. Sialic acid in milk powder was released by acid hydrolysis, then had a derivative reaction with ophenylenediamine. The separation of sialic acid derivatives was achieved on C18column with gradient elution, and quantitated by external standard method with fluoresce detector. Sources of uncertainty in the whole measurement process were investigated. The uncertainty introduced by each factor was calculated and synthesized. The extended uncertainty was given. When the determination result of sialic acid in milk powder was 2 586 mg/kg, the expand uncertainty was 153 mg/kg(k=2). The main factors affecting the uncertainty evaluation of sialic acid include the preparation of standard working solution, the constant volume of sample and the repeatability of measurement. The scientificity and accuracy of measurement results can be improved by performing normalization operations, preparing suitable standard solution, and increasing the number of parallel sample measurements.

关 键 词：测量不确定度 唾液酸 乳粉 液相色谱法 

分 类 号：O657.7[理学—分析化学]