国家标准GB/T 21316—2007测定动物源性食品中磺胺类药物残留量的不确定度评定

Uncertainty Evaluation for Determination of Sulfonamide Residues in Animal-derived Foods by National Standard GB/T 21316-2007

对国家标准GB/T 21316-2007测定动物源性食品中磺胺类药物残留量的测量不确定度进行评定。根据《测量不确定度评定与表示》(JJF 1059.1-2012)和《化学分析中不确定度的评估指南》(CNAS-GL006:2019)中的规定,建立测定鳗鱼肉中磺胺残留量测定的数学模型,根据测量不确定度的来源,以磺胺甲基嘧啶为例,对各个不确定度分量进行评定和分析。评定结果表明,当样品磺胺甲基嘧啶含量检测结果为10.4μg/kg时,扩展不确定度为3.4μg/kg。不确定度按照从大到小排列,依次为标准曲线最小二乘法拟合、测量重复性、回收率、标准溶液制备、LC/MS/MS定量重复性、样品定容、样品称量。

The uncertainty of determination of sulfonamide residues in animal-derived foods by GB/T 21316-2007 was evaluated.According to "Evaluation and Expression of Uncertainty in Measurement"(JJF 1059.1-2012)and "Guidance on Quantifying Uncertainty in Chemical Analysis"(CNAS-GL006:2019),a mathematical model for determination of sulfonamide residues in eel meat was established.Based on the sources of the measurement uncertainty,each uncertainty of sulfamethazine as an example was evaluated and analyzed.The evaluation results showed that the extended uncertainty was 3.4 μg/kg when the test result of sulfamethazine content in samples was 10.4 μg/kg.The uncertainty was arranged in order from large to small,which were least squares calibration,measurement repeatability,recovery rate,standard solution preparation,LC/MS/MS quantitative repeatability,sample volume determination and sample weighing.