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JJF1059.1-2012《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100μg/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。
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.
作者
孙婧
刘晓海
SUN Jing;LIU Xiao-Hai(Mengniu Dairy products Wuhan Co.,Ltd.,Wuhan 430040,China)
出处
《食品安全质量检测学报》
CAS
2018年第19期5228-5234,共7页
Journal of Food Safety and Quality
关键词
不确定度
高效液相色谱法
甲砜霉素
牛奶
uncertainty
high performance liquid chromatography
thiamphenicol
milk