利用超高效液相色谱-串联质谱法测定牛奶中氮氨菲啶残留量,并根据建立的数学模型评定该方法不确定度的各分量值。样品经乙腈溶液溶解,过C18小柱净化,超高效液相色谱-串联质谱测定,外标法定量。评定结果表明,标准曲线引入、回收率实验产生不确定度分量最大。当牛奶中氮氨菲啶含量为0.017 8 mg/kg时,其扩展不确定度为0.007 8 mg/kg(k=2)。
The ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was used to determine the isometamidium residues in milk, and the mathematic model based on this method was built for the evaluation of its uncertainty. The sample was firstly dissolved in acetonitrile solution, purified by C18 column, and then determined by ultra performance liquid chromatography-tandem mass spectrometry. Finally, was quantified by external standard method. The evaluation results showed that the uncertainty components had been mainly impacted by the introduction of the standard curve and recovery experiment. The expanded uncertainty was 0.007 8 mg/kg (k=2) when the content of phenanthridine in milk was 0.017 8 mg/kg.
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