液质联用测定水产品中硝基呋喃类代谢物残留量的不确定度评定

Uncertainty evaluation in determination of nitrofuran metabolites residues in aquatic product by liquid chromatography-tandem mass spectrometry

目的采用液相色谱串联质谱法对水产品中硝基呋喃类代谢物的残留量进行测量不确定度评定。方法根据农业部783号公告-1-2006的前处理方法进行处理,根据JJF 1059.1-2012《测量不确定度的评定与表示》等相关理论,通过建立数学模型,对测量结果的各不确定度来源进行分析和量化。结果当硝基呋喃类代谢物的添加水平为2.0 ng/m L时,4种硝基呋喃类代谢物结果可表示为呋喃西林代谢物(2.114±0.114)ng/m L,k=2;呋喃妥因代谢物(2.162±0.124)ng/m L,k=2;呋喃它酮代谢物(1.880±0.107)ng/m L,k=2;呋喃唑酮代谢物(2.076±0.097)ng/m L,k=2。结论在确定的实验条件下,本方法的不确定度主要来自于仪器设备测试引起的峰面积的变化,呋喃西林代谢物和呋喃妥因代谢物方法的回收率也是一个主要影响因素。

Objective To establish a mathematical model of uncertainty evaluation of nitrofuran metabolites residues in aquatic product by high performance liquid chromatography-tandem mass spectrometry. Methods Based onThe Ministry of Agriculture announcementNo.783-1-2006, JJF 1059.1-2012 Evaluation and expression of uncertainty in measurement and other theories, a mathematical model was constructed and each component of uncertainty in the whole measuring process was analyzed and quantified.ResultsThe results showed that when the spiked level was 2.0 ng/mL, the expanded uncertainty wasUSEM(2.114±0.114) ng/mL,k=2;UAHD(2.162±0.124) ng/mL,k=2;UAMOZ(1.880±0.107) ng/mL,k=2; andUAOZ(2.076±0.097) ng/mL, k=2.Conclusion Under determined experimental conditions, the major uncertainty sources were the area of determination and the recovery of method.