UPLC-MS-MS法测定花生中黄曲霉毒素的不确定度评定

摘要

对应用超高液相色谱串联质谱法测定花生中4种黄曲霉毒素含量的测量不确定度进行评定.根据JJF 1135-2005《化学分析测量不确定度评定》和JJF 1059.1-2012《测量不确定度评定与表示》中的有关规定和基本程序,建立测定花生中4种黄曲霉毒素含量的数学模型,依据影响测量不确定度的来源,对各个不确定度分量进行评定和分析,给出了1 μg/kg的检测水平下,超高液相色谱串联质谱法测定花生中4种黄曲霉毒素测定结果的扩展不确定度.通过比较各个分量不确定度,发现实验过程中最小二乘法拟合带来的不确定度影响最大.%The uncertainty of four aflatoxins determination in Peanut was evaluated by ultra-performance liquid chromatography tandem mass spectrometry was evaluated. According to the relevant provisions and basic procedures of JJF 1135-2005"Evaluation of Measurement Uncertainty in Chemical Analysis"and JJF 1059.1-2012"Evaluation and Expression of Measurement Uncertainty",a mathematical model for determination of four aflatoxins in peanut was established. Based on the sources of the measurement uncertainty, each uncertainty were evaluated and analyzed, respectively. Extended uncertainty of four aflatoxins determination results in peanut was determined by ultr-performance liquid chromatography tandem mass spectrometry(UPLC-MS-MS) at the detection level of 1μg/kg. Compared with the uncertainty of each component, it is found that the uncertainty caused by least square fitting in the experiment has the greatest influence.