鸡蛋中多西环素残留测定不确定度评定

Uncertainty Evaluation for The Determination of Doxycycline Residues in Eggs

关键词:  高效液相色谱-串联质谱法  鸡蛋  多西环素  不确定度

Key words:  HPLC-MS/MS  Eggs  Doxycycline  Uncertainty

摘要:

评定了高效液相色谱串联质谱法测定鸡蛋中多西环素残留量的不确定度，通过建立数学模型，对高效液相色谱-串联质谱法测定鸡蛋中多西环素残留量进行不确定度评定，分析不确定度来源，评价其对测定结果不确定度的相对贡献，并计算合成不确定度，最终得到鸡蛋中多西环素残留量的扩展不确定度。结果显示，鸡蛋中多西环素残留量为9.18 μg/kg，在95%的置信区间下，合成不确定度0.0583，扩展不确定度为0.1166（k=2），最终结果应表示为9.18±1.07 μg/kg，实验过程中不确定度主要来源于工作曲线的配制过程，测量重复性和回收率。本研究可为以后的检测工作提供可行性建议。

Abstract:

To evaluate the uncertainty of the determination of doxycycline residues in eggs by high performance liquid chromatography tandem mass spectrum (HPLC-MS/MS), we established a mathematical model, the uncertainty assessment of the testing of the doxycycline residues in eggs by HPLC-MS/MS was carried out. The cause of uncertainty was analyzed, and its relative contribution to the uncertainty in the testing process was evaluated, combined uncertainty was calculated, and the expanded uncertainty for doxycycline residues in eggs was got finally. The result shows that doxycycline residue in eggs was 9.18 μg/kg. Under the 95% confidence interval, the combined uncertainty was 0.0583, and the expanded uncertainty was 0.1166 (k=2), the final result should be expressed as 9.18±1.07 μg/kg, The uncertainty in the testing process is mainly comes from the preparation process of the working curve, measurement repeatability and recovery rate. This study can provide practical suggestions for future testing work.