饮料中甜蜜素含量测定的不确定度评定

Uncertainty of Sodium Cyclamate Content in Beverages Tested by UPLC-MS/MS

目的建立超高效液相色谱—串联质谱法测定饮料中甜蜜素含量不确定度评定的数学模型,对各不确定度分量进行量化与评估。方法根据《测量不确定度评定与表示》(JJF 1059.1-2012),分析测定过程各不确定度来源,计算各分量,评估饮料中甜蜜素含量测定的不确定度。结果当饮料中甜蜜素含量为0.11μg/kg,置信概率为95%,包含因子k=2,其扩展相对不确定度为0.06μg/kg。结论通过对不确定度的分析,发现标准曲线拟合残差是超高效液相色谱—串联质谱法测定饮料中甜蜜素含量不确定度的主要来源,并由此提出了质量控制改进方法。

Objectives A mathematical model was established to assess the uncertainty of sodium cyclamate content in beverages tested by ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS / MS）. Methods Based on JJF1059. 1- 2012 about evaluation and expression of uncertainty inmeasurement,the sources of uncertainty for determination were analyzed and each component of uncertainty was evaluated. Results When the content of sodium cyclamate in beverages was 0. 11 μg / kg,the confidence probability was 95%,comprising a factor of k = 2,its extended relative uncertainty was 0. 06 μg / kg. Conclusion Based on the analysis of uncertainty,it was found that the fitting residual error of standard curve was the main source of uncertainty; and then improved methods for quality control were put forward.