奶粉中香兰素甲基香兰素和乙基香兰素UPLC-MS/MS法的不确定度评定

Uncertaintyevaluation of Vanillin Methylvanillin and Ethylvanillin in Milk Powder by UPLC-MS/MS

评定UPLC-MS/MS法测定奶粉中香兰素、甲基香兰素、乙基香兰素含量的不确定度。分析测定过程中影响测量值的不确定度因素,根据检测方法建立的不确定度数学模型,进行添加回收测试并计算分析各个标准不确定度的分量。在奶粉的香兰素、甲基香兰素和乙基香兰素含量测定中当目标物含量为100.0μg/kg时,其结果含量分别为香兰素100.0±7.1μg/kg,甲基香兰素100.0±7.6μg/kg,乙基香兰素100.0±8.4μg/kg,k=2。研究表明,标准溶液称量稀释过程、标准工作曲线拟合、重复性测量和测量回收率因素对测定结果的准确度影响比较显著,在检测过程需要多加关注。

To evaluate the uncertainty of determination of vanillin,methylvanillin and ethylvanillin in milk powder by UPLC-MS/MS.Analyzed the uncertainty factors affecting the measured value in the determination process,and establish a mathematical model of uncertainty evaluation,calculate the component of each standard uncertainty by adding test.When the contents of vanillin、methylvanillin and ethylvanillin in milk powder were 100.0μg/kg,the determination results were 100.0±7.1μg/kg,100.0±7.6μg/kg and 100.0±8.4μg/kg,k=2.The results showed that preparation process of standard solution,fitting standard working curves,repeatability measurement,measured recovery had a significant impact on the accuracy of the determination results,so we should pay more attention in the detection process.