液质联用法测定香肠中氯霉素的不确定度评定

Evaluation of Uncertainty in the Determination of Chloramphenicol in Sausage by Liquid Chromatography-Mass Spectrometry Method

本文采用高效液相色谱-质谱法对香肠中的氯霉素含量进行了测试,为进一步证明该测量方法结果的准确性和科学性,建立了相应的数学模型对氯霉素含量测试的不确定度进行考察评定。通过分析测量过程中产生的不确定度,计算相对合成不确定度和扩展不确定度,得到了香肠中氯霉素测定结果的不确定度报告。结果显示,该方法测得香肠中氯霉素残留量为0.98μg·kg^(-1),扩展不确定度为0.17μg·kg^(-1)。其中,影响不确定度的重点因素主要为标准储备液、中间液和标准曲线测试液的配制、标准曲线的拟合和仪器校准。

In this paper,the chloramphenicol content in sausage was measured by high performance liquid chromatography-mass spectrometry,in order to further prove the accuracy and scientificity of the measurement method,a corresponding mathematical model was established to evaluate the uncertainty of chloramphenicol content test.The uncertainty report of chloramphenicol determination in sausage was obtained by analyzing the uncertainty generated in the measurement process,calculating the relative synthetic uncertainty and the extended uncertainty.The results showed that the chloramphenicol residue in sausage was 0.98μg·kg^(-1),the expanded uncertainty is 0.17μg·kg^(-1).Among them,the key factors affecting the uncertainty are mainly the preparation of standard stock solution,intermediate solution and standard curve test solution,the fitting of standard curve and the calibration of instrument.