乳业科学与技术 ›› 2025, Vol. 48 ›› Issue (5): 0-0.

• 分析检测 •    

气相色谱-质谱联用测定奶粉中三聚氰胺残留量的不确定度评价

张婷,王舒婷,李嘉,车彦卓,程用斌   

  1. 陕西省农业检验检测中心
  • 收稿日期:2025-06-09 修回日期:2025-07-29 出版日期:2025-09-01 发布日期:2025-10-05
  • 通讯作者: 程用斌

Uncertainty evaluation of determination of melamine residue in milk powder by gas chromatography-mass spectrometry

  • Received:2025-06-09 Revised:2025-07-29 Published:2025-09-01 Online:2025-10-05

摘要: 目的 评定气相色谱-质谱联用测定奶粉中三聚氰胺残留量的不确定度。方法 依据GB/T 22238-2008《原料乳与乳制品中三聚氰胺检测方法》中的第三法:气相色谱-质谱联用法,结合CNAS-GL006《化学分析中的不确定度评估指南》,建立数学模型,对实验过程中不确定度来源进行分析和评定,并计算各不确定度得到的合成标准不确定度。结果 当样品中三聚氰胺含量为2.09mg/kg时,其扩展不确定度为0.182mg/kg(k=2)。结论 检测结果的不确定度来源于以下三个分量样品定容、标准溶液配制和曲线拟合以及实验过程的回收率。

关键词: 三聚氰胺, 气相色谱-质谱联用法, 不确定度评定

Abstract: Objective To evaluate the uncertainty of determination of melamine residue in milk powder by gas chromatography-mass spectrometry. Methods According to the third method in GB/T 22238-2008 《Methods for the Determination of Melamine in Raw Milk and Dairy Products》: Gas chromatography-mass spectrometry, combined with CNAS-GL006 Uncertainty Evaluation Guide for Chemical Analysis, a mathematical model was established to analyze and evaluate the sources of uncertainty during the experiment, and the synthetic standard uncertainty obtained from each uncertainty was calculated. Results When the content of melamine was 2.09mg/kg, the extended uncertainty was 0.182mg/kg (k=2). Conclusions The uncertainty of test results mainly comes from sample recovery, repeatability, standard solution preparation and curve fitting.

Key words: Melamine, Gas chromatography-mass spectrometry, Evaluation of uncertainty