UHPLC-MS/MS法测定鞋材中壬基酚的不确定度分析

Uncertainty Analysis of Nonylphenol in Footwear Materials Determined by UHPLC-MS/MS

采用超高效液相色谱-串联质谱法测定鞋类部件中烷基苯酚和邻苯基苯酚残留量,以壬基酚为代表建立不确定度测量模型。通过对样品称量、定容、重复性测定、标准物质、工作曲线绘制及拟合、仪器校准等测量不确定来源进行评定、合成,结果表明当试样中壬基酚含量为5.07 mg/kg时,扩展不确定度为0.81 mg/kg(k=2),其中仪器校准和标准工作曲线绘制是不确定度的主要来源。

The residues of alkylphenol and o-phenylphenol in footwear were determined by ultra high performance liquid chromatography tandem-mass spectrometry(UHPLC-MS/MS),and the uncertainty analysis model was established by using nonylphenol as the representative.Through the evaluation and synthesis of measurement uncertainty sources such as sample weighing,constant volume,repeatability determination,standard material,working curve drawing and fitting,instrument calibration and so on,the results showed that when the content of nonylphenol in the sample was 5.07 mg/kg,the expanded was 0.81 mg/kg(k=2),and the main source of uncertainty was instrument calibration and standard working curve drawing.