鸡肉中强力霉素残留测定不确定度评定

Uncertainty evaluation for the determination of doxycycline residue in chicken

中文关键词:  鸡肉  强力霉素  残留  不确定度

英文关键词:chicken  doxycycline  residue  uncertainty

中文摘要:

      目的 对液相色谱-质谱/质谱法测定鸡肉中强力霉素残留的不确定度进行评定, 找出影响检测结果准确性的关键因素, 从而提高检测结果准确性。方法 按照GB/T 21317-2007《动物源性食品中四环素类兽药残留量检测方法 液相色谱-质谱/质谱法与高效液相色谱法》对鸡肉中强力霉素残留量进行测定。通过建立数学模型, 对影响测量结果的不确定度来源如标准物质的纯度、标准物质的称量、标准曲线的配制、样品的称量、样品的制备、标准曲线的拟合、样品测量重复性等因素进行分析和评定。结果 鸡肉中强力霉素残留量为123.8 μg/kg, 扩展不确定度为8.9 μg/kg, 测定结果表示为: X=(123.8±8.9) μg/kg(k=2)。结论 样品测量重复性和标准曲线绘制是本次测定测量不确定度的主要来源, 在检测过程中应加以控制。

英文摘要:

      Objective To evaluate the uncertainty for the determination of doxycycline residue in chicken by liquid chromatography-mass spectrometry/mass spectrometry(LC-MS/MS), and identify the key factors affecting the accuracy of detection results and improve the accuracy of detection results. Methods The doxycycline residue in chicken was determined according to GB/T 21317-2007 Determination of tetracyclines residues in food of animal orgin-LC-MS/MS method and HPLC method. The uncertainty sources affecting the measurement results, such as the purity of the standard substance, the weighing of the standard substance, the preparation of the standard curve, the weighing of the sample, the preparation of the sample, the fitting of the standard curve, the repeatability of the sample measurement were analyzed and evaluated by establishing a mathematical model. Results The doxycycline residue in the chicken was 123.8 μg/kg, the extended uncertainty was 8.9 μg/kg, and the determination results were expressed as X=(123.8±8.9) μg/kg (k=2). Conclusion The sample measurement repeatability and the standard curve preparation are the main sources of the uncertainty evaluation, and should be controlled during testing.