LC-MS/MS测定牛奶中四环素残留量的不确定度评定

Uncertainty Evaluation for Determination of Tetracycline Residues in Milk by LC-MS/MS

目的:分析评定《食品安全国家标准动物性食品中四环素类、磺胺类和喹诺酮类药物残留量的测定液相色谱-串联质谱法》(GB 31658.17—2021)检验方法中牛奶兽药残留四环素测量结果的不确定度。方法:根据《测量不确定度评定与表示》(JJF 1059.1—2012)、参照GB 31658.17—2021方法测定牛奶中四环素含量。通过对牛奶中四环素残留量检测过程中相关不确定度分量进行数学建模,分析评定牛奶中兽药残留四环素测量结果的不确定度。结果:牛奶中四环素测量的扩展不确定度为1.197 4μg·kg-1,牛奶中四环素残留量测定结果为(41.58±1.197 4)μg·kg(k=2)。结论:在四环素的检测中,可通过控制标准溶液的配制过程、增加标准曲线溶液的测量次数和提高仪器的稳定性和灵敏度等方法来提高四环素检测结果的准确性和可靠性。

Objective:To analyze and evaluate the uncertainty of the measurement results of tetracycline residue in milk in GB 31658.17—2021 test method.Method:The content of tetracycline in milk was determined according to JJF 1059.1—2012 and GB 31658.17—2021.The uncertainty of the measurement result of tetracycline residue in milk was analyzed and evaluated by mathematical modeling of the correlation uncertainty in the detection process of tetracycline residue in milk.Result:The extended uncertainty of the measurement of tetracycline in milk was 1.1974μg·kg^(-1),and the residual determination of tetracycline in milk was(41.58±1.1974)μg·kg^(-1)(k=2).Conclusion:The accuracy and reliability of tetracycline detection can be improved by controlling the preparation process of the standard solution,increasing the measurement times of the standard curve solution and improving the stability and sensitivity of the instrument.