UPLC-MS/MS法测定虾肉中氯霉素残留量的不确定度分析

Uncertainty analysis of determination of chloramphenicol residue in shrimp by UPLC-MS/MS method

采用超高效液相色谱-串联质谱(UPLC—MS/MS)法测定Fapas能力验证项目虾肉中氯霉素的残留量,并进行不确定度评定,给出了不确定度。先建立了测定虾肉中氯霉素残留量的不确定度的数学模型,再对不确定度来源进行分析。通过对不确定度分量进行量化和合成,得出当虾肉中氯霉素残留量为0.820 8μg/kg时,其扩展不确定度为0.146 2μg/kg(k=2),结果符合Fapas能力验证指定范围。评定结果表明,UPLC—MS/MS法测定虾肉中氯霉素试验过程中,样品称量、样品提取、校准曲线的配制、质谱测定、校准曲线的拟合等过程都会引入不确定度,其中,标准系列溶液配制和标准曲线的拟合引入的不确定度最大。

In this paper,the Fapas ability was used to verify the chloramphenicol residues in shrimp meat by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）,and the uncertainty was evaluated.Uncertainty was given.First,a mathematical model for determining the uncertainty of chloramphenicol residues in shrimp was established, and then the source of uncertainty was analyzed.The uncertainty of the uncertainty was0.146 2μg/kg（k = 2）when the chloramphenicol residues in the shrimp were 0.820 8μg/kg,and the results were in accordance with the Fapas ability test.Specify the scope.The results showed that the UPLC-MS/MS method was used to determine the uncertainty of the process of determination of chloramphenicol in shrimp,sample weighing,sample extraction,calibration curve,mass spectrometry and calibration curve etc were the major infact for uncertainty.The standard series solution formulation and the fitting of the standard curve were introduced with the greatest uncertainty.