液相色谱串联质谱法测定玉米中伏马毒素的不确定度评定

Assessment of the Uncertainty of Fumonisins Determination in Corn by Liquid Chromatography Tandem Mass Spectrometry

目的:评定同位素内标高效液相色谱-串联质谱法测定玉米中伏马毒素的不确定度。方法:采用HPLC-MS/MS结合同位素内标法测定玉米中伏马毒素含量,建立数学模型,对实验测量结果重复性、拟合标准曲线、前处理方法等不确定度来源进行分析和评定,得出合成标准不确定度和扩展不确定度。结果:应用建立的方法检测玉米中伏马毒素(FB、FB、FB)的含量,分别为81.68μg·kg^(-1)、59.79μg·kg^(-1)、68.62μg·kg^(-1),扩展不确定度分别为5.60μg·kg^(-1)、3.82μg·kg^(-1)、3.61μg·kg^(-1)(k=2)。结论:该方法测定玉米中伏马毒素含量的不确定度总体较小,最大测量不确定度由配制标准溶液引入,提醒需在实际操作过程中准确配制标准溶液。

Objective: To evaluate the uncertainty of determination of fumonisins in corn by high performance liquid chromatography-tandem mass spectrometry with isotope internal standard. Method: HPLC-MS/MS method combined with isotope internal standard was used to determine the content of fumonisins in corn. A mathematical model was established to analyze and evaluate sources of uncertainty such as measurement repeatability, standard curve, and sample pretreatment.Certainty and expanded uncertainty were finally obtained. Result: The contents of fumonisins(FB, FB, FB) in corn were detected as 81.68 μg·kg^(-1), 59.79 μg·kg^(-1), 68.62 μg·kg^(-1), and their expanded uncertainties were 5.60 μg·kg^(-1), 3.82 μg·kg^(-1),3.61 μg·kg^(-1)(k=2). Conclusion: The method has an overall small uncertainty in the determination of fumonisins content in maize, with the maximum measurement uncertainty introduced by the fitting of the standard solution which requiring attention during actual operation.