高效液相色谱-串联质谱法测定牛奶中3种磺胺类药物残留不确定度的评定

Uncertainty evaluation of three sulfonamides residues in milk by high per-formance liquid chromatography-tandem mass spectrometry

中文关键词:  磺胺吡啶  磺胺噻唑  磺胺甲基异恶唑  高效液相色谱-串联质谱法  牛奶  不确定度

英文关键词:sulfapyridin  sulfathiazole  sulfamethoxazole  liquid chromatography-tandem mass spectrometry  milk  uncertainty

中文摘要:

      目的 采用高效液相色谱-串联质谱法对牛奶中磺胺吡啶、磺胺噻唑和磺胺甲基异恶唑残留的不确定度进行评估。方法 建立测定牛奶中磺胺吡啶、磺胺噻唑和磺胺甲基异恶唑含量不确定度的数学模型, 确定不确定度来源并对其评定。结果 当牛奶中磺胺吡啶含量为5.09 μg/kg 时, 其扩展不确定度为0.62 μg/kg (k=2); 当牛奶中磺胺噻唑含量为8.62 μg/kg 时, 其扩展不确定度为0.71 μg/kg (k=2); 当牛奶中磺胺甲基异恶唑含量为10.15 μg/kg 时, 其扩展不确定度为0.81 μg/kg(k=2)。其中, 测量重复性和标准曲线对不确定度的影响最大。 结论 影响检测结果不确定度的主要因素为样品测量的重复性、标准曲线拟合和样品的前处理过程。

英文摘要:

      Objective To establish a mathematical model of uncertainty evaluation of sulfapyridine, sulfathiazole and sulfamethoxazole in milk by high performance liquid chromatography-tandem mass spectrometry method. Methods To establish a mathematical model for determination of sulfapyridine, sulfathiazole and sulfamethoxazole uncertainty in milk. The sources of uncertainty of the whole determination procedure were analyzed and the combined uncertainty was finally obtained. Results The expanded uncertainty of 5.09 μg/kg (k=2) with 0.62 μg/kg of the content of sulfapyridin was derived. The expanded uncertainty of 8.62 μg/kg (k=2) with 0.71 μg/kg of the content of sulfathiazole was derived. The expanded uncertainty of 10.15 μg/kg (k=2) with 0.81 μg/kg of the content of sulfamethoxazole was derived. The major sources of uncertainty of measurement include the repeatability of detection and the curve fitting. Conclusion The major uncertainty sources were standard curve fitting; measurement repeatability and sample pretreatment.