高效液相色谱法测定灭菌乳中糠氨酸的不确定度评定

Uncertainty evaluation for the determination of furosine in sterilized milk by high performance liquid chromatography

中文关键词:  灭菌乳  糠氨酸  不确定度  高效液相色谱法

英文关键词:sterilized milk  furosine  uncertainty  high performance liquid chromatography

中文摘要:

      目的 评定高效液相色谱法测定灭菌乳中糠氨酸含量结果的不确定度。方法 依据NY/T939-2016《巴氏杀菌乳和UHT灭菌乳中复原乳的鉴定》测定灭菌乳中糠氨酸的含量, 建立高效液相色谱法测定灭菌乳中糠氨酸含量的不确定度评定的数学模型, 全面分析实验过程中各不确定度的来源, 并对各不确定度进行分量量化及合成, 计算灭菌乳中糠氨酸的合成标准不确定度及扩展不确定度。结果 灭菌乳中糠氨酸含量为151.0 mg/100 g蛋白质时, 测量结果的扩展不确定度为5.8 mg/100 g蛋白质(k=2)。结论 溶液配制、蛋白质检测终点判断、色谱峰峰面积积分、样品重复性实验、加标回收率实验引入的不确定度对糠氨酸总不确定度贡献较大。

英文摘要:

      Objective To evaluate the uncertainty of determination of furosine in sterilized milk by high performance liquid chromatography. Methods According to NY/T939-2016 Identification of restored milk in pasteurized milk and UHT sterilized milk, the content of furfurine in the sterilized milk was determined. A mathematical model for uncertainty evaluation of determination of furosine in sterilized milk by high performance liquid chromatography was established, the source of each uncertainty in the experiment was analyzed comprehensively, the components of each uncertainty were quantified and synthesized, and the standard uncertainty and extended uncertainty of the synthesis of furosine in sterilized milk were calculated. Results When the content of furosine in sterilized milk was 151.0 mg/100 g protein, the expanded uncertainty of measurement results was 5.8 mg/100 g protein (k=2). Conclusion The uncertainties introduced by solution preparation, protein detection endpoint judgment, chromatographic peak area integration, sample repeatability experiment, and standard addition recovery experiment contribute a lot to the total uncertainty of furosine.