液相色谱-串联质谱法测定鸡肉中氯霉素的不确定度评定

Uncertainty evaluation of determination of chloramphenicol in chicken by liquid chromatography tandem mass spectrometry method

采用液相色谱-串联质谱法测定鸡肉中的氯霉素含量,分析不确定度来源,并对不确定度进行评定。通过10次重复测定,考察A类不确定度;通过对实验过程的全面分析,从标准物质、样品称量、定容、校准曲线拟合过程,评价B类不确定度;取置信水平P=95%,k=2,最终给出液相色谱串联质谱法测定鸡肉中氯霉素含量的扩展不确定度。通过分析,引起本实验室过程不确定度的主要因素为标准物质配制、校准曲线拟合、标准物质纯度,以及实验重复性,样品称量引起的不确定度可忽略。此研究可提升实验室质量稳定性,并为同行业检测人员进行不确定度评定工作提供有效理论参考。

The liquid chromatography tandem mass spectrometry method was adopted,and the content of chloramphenicol in chicken was determined,and the source of uncertainty was analyzed,and the uncertainty was evaluated.Through ten repeated determinations,the uncertainty of class A was investigated.Through the comprehensive analysis of the experimental process,the uncertainty of class B was evaluated from the standard material,sample weighing,constant volume and calibration curve fitting process.The P=95%and K=2 were taken as confidence level.Finally,the extended uncertainty of the determination of chloramphenicol in chicken by liquid chromatography tandem mass spectrometry method was given.Through analysis,the main factors causing the uncertainty of process in our laboratory were the preparation of standard materials,calibration curve fitting,purity of standard materials and experimental repeatability.The uncertainty caused by sample weighing could be ignored.This study could improve the quality stability of laboratory,and it provided an effective reference for the uncertainty assessment work of the same industry testing personnel.