高效液相色谱法测定巴氏杀菌乳中糠氨酸含量的不确定度评定

Uncertainty Evaluation for the Determination of Furosine in Milk by HPLC

[目的]对高效液相色谱法测定巴氏杀菌乳中糠氨酸含量的不确定度进行评定。[方法]依据《NY/T939—2016巴氏杀菌乳和UHT灭菌乳中复原乳的鉴定》测定巴氏杀菌乳中糠氨酸的含量。通过建立数学模型,全面分析试验过程中各不确定度的来源,并对其进行量化评定,计算合成相对标准不确定度和扩展不确定度。[结果]当牛奶中糠氨酸含量为7.3 mg/100 g蛋白质时,测量结果的扩展不确定度为0.4 mg/100 g蛋白质(k=2)。[结论]方法中测量不确定度的主要来源为糠氨酸标准物质称量、标准工作液的配制、标准曲线的拟合和样品水解液中蛋白质含量测定终点判定。

[Objective]Evaluate the uncertainty of the determination of furosine in pasteurized milk by HPLC.[Method]According to NY/T 939-2016,the content of furosine in pasteurized milk was determined.Through the establishment of a mathematical model,the sources of various uncertainties in the experimental process were comprehensively analyzed and quantitatively evaluated,and the relative standard uncertainty and expanded uncertainty of the synthesis of furosine in pasteurized milk were calculated.[Result]When the content of furosine in pasteurized milk was 7.3 mg/100 g protein,the expanded uncertainty of the measurement results was 0.4 mg/100 g protein(k=2).[Conclusion]The main sources of measurement uncertainty of this method include the weighing of furosine reference material,the preparation of standard working solution,the fitting of standard curve and the determination of the end point of protein content in sample hydrolysate.