液相色谱-质谱质谱法测定鸭蛋中氟苯尼考残留量不确定度评定
目的 对液相色谱-质谱/质谱法测定鸭蛋中氟苯尼考残留的不确定度进行评定, 确定影响检测结果准确性的关键因素, 提高检测结果准确性。方法 按照GB/T 22338-2008《动物源性食品中氯霉素类药物残留量测定》液相色谱-质谱/质谱法对鸭蛋中氟苯尼考残留量进行测定。依据CNAS-GL006:2018《化学分析中不确定度的评估指南》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了分析和评定。结果 鸭蛋中氟苯尼考残留量为210 μg/kg, 扩展不确定度为18 μg/kg, 测定结果表示为: X=(210± 18) μg/kg(k=2)。结论 样品测量重复性和标准曲线配制是本次测定不确定度的主要来源, 在检测过程中应加以控制。
Objective To evaluate the uncertainty for the determination of florfenicol residue in duck eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS), determine the key factors affecting the accuracy of the detection results, and improve the accuracy of the detection results. Methods Florfenicol residues in duck eggs were determined by LC-MS/MS according to GB/T 22338-2008 Determination of chloramphenicol residues in food of animal origin. According to CNAS-GL006:2018 Guide for evaluation of uncertainty in chemical analysis, a mathematical model was established to analyze and evaluate the sources of uncertainty such as purity of reference materials, weighing of reference materials, preparation of standard curves, weighing of samples, preparation of samples, fitting of standard curves, repeatability of sample measurement, etc. Results The florfenicol residue in the duck egg was 210 μg/kg and the extended uncertainty was 18 μg/kg. The determination results were expressed as X=(210±18) μg/kg (k=2). Conclusion The repeatability of sample measurement and the preparation of standard curve are the main sources of measurement uncertainty, which should be controlled in the detection process.
标题：液相色谱-质谱质谱法测定鸭蛋中氟苯尼考残留量不确定度评定
英文标题：Uncertainty evaluation for the determination of florfenicol residue in duck eggs by liquid chromatography-tandem mass spectrometry
作者：
辛丽娜 广西-东盟食品检验检测中心
黄燕红 广西-东盟食品检验检测中心
梁飞燕 广西-东盟食品检验检测中心
中文关键词:鸭蛋,氟苯尼考,残留,不确定度,液相色谱-质谱/质谱法,
英文关键词:duck eggs,florfenicol,residue,uncertainty,liquid chromatography-tandem mass spectrometry,
发表日期：2020-05-19
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