高效液相色谱法测定牛奶中甲砜霉素残留量的不确定度评定

Uncertainty evaluation of the determination of thiamphenicol residues in milk by high performance liquid chromatography

中文关键词:  不确定度  高效液相色谱法  甲砜霉素  牛奶

英文关键词:uncertainty  high performance liquid chromatography  thiamphenicol  milk

中文摘要:

      目的 评定高效液相色谱法(high performance liquid chromatography, HPLC)测定牛奶中甲砜霉素残留量的不确定度。方法 根据GB29689-2013《食品安全国家标准牛奶中甲砜霉素残留量的测定高效液相色谱法》和JJF 1059.1-2012《测量不确定度评定与表示》, 建立分析HPLC测定牛奶中甲砜霉素残留量不确定度的数学模型, 通过对整个测定过程中的不确定度来源进行分析和合成, 运用最小二乘法对甲砜霉素标准曲线拟合的不确定度进行评定。结果 当取样量为5.00 g, k=2(95%置信度)时, 测得甲砜霉素理论含量为100 μg/kg的牛奶中甲砜霉素的残留量为(91.4±2.2) μg/kg。结论 本方法的主要不确定来源为标准溶液浓度、标准曲线拟合以及试样测量重复性。

英文摘要:

      Objective To evaluate the uncertainty of thiamphenicol residues in milk by high performance liquid chromatography (HPLC). Methods According to GB29689-2013 National standard for food safety-Determination of thiamphenicol residues in milk-High performance liquid chromatography and JJF 1059.1-2012 Measurement and expression of measurement uncertainty, the mathematical model for the determination of the uncertainty of thiamphenicol residues in milk by HPLC was established. The uncertainty of the fitting of the standard curve of thiamphenicol was assessed by least squares method by analyzing and synthesizing the sources of uncertainty throughout the assay. Results When the sample was 5.00 g, k=2 (95% confidence), the result of determination of the residual amount of thiamphenicol in milk with a theoretical content of thiamphenicol of 100 μg/kg was (91.4± 2.2) μg/kg. Conclusion The main sources of uncertainty for this method include standard solution concentration, standard curve fit, and sample measurement repeatability.