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

作　　者：李涛 周艳华[2] 杨滔 孙桂芳 

机构地区：[1]湖南省食品质量监督检验研究院,湖南长沙410111 [2]长沙环境保护职业技术学院,湖南长沙410004

出　　处：《食品与机械》2017年第7期61-64,99,共5页Food and Machinery

基　　金：湖南省自然科学基金项目(编号:2017JJ5062)

摘　　要：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.

关 键 词：超高效液相色谱-串联质谱(UPLC—MS/MS) 虾 氯霉素 不确定度 Fapas 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]