HPLC-MS/MS测定动物性食品中氟苯尼考及氟苯尼考胺残留量结果的不确定度评定

Evaluation of Uncertainty in the Determination of Florfenicol and Florfenicol Amine Residues in Animal Foods by HPLC-MS/MS

评价了采用液相色谱串联质谱法测定猪肉中氟苯尼考及氟苯尼考胺残留量的不确定度。通过对不确定度来源进行分析,构建了不确定度评定数学模型,并对影响不确定度的各个因素进行考察,计算各个分量的标准不确定度以及扩展不确定度,最终得出不确定度结果。结果表明,当猪肉中氟苯尼考含量为7.6μg·kg^(-1)时,其扩展不确定度为1.2μg·kg^(-1)(k=2);氟苯尼考胺含量为7.0μg·kg^(-1)时,其扩展不确定度为1.1μg·kg^(-1)(k=2)。测定结果的不确定度主要来源于混标系列工作液的配制过程。本研究可对实验室采用GB 31658.5—2021测定猪肉中氟苯尼考及氟苯尼考胺的过程和结果进行有效质量控制提供重要参考。

The uncertainty of determination of florfenicol and florfenicol amine residues in animal food by liquid chromatography-tandem mass spectrometry is evaluated.By analyzing the sources of uncertainty,the mathematical model is established,and the factors affecting the uncertainty are investigated,the standard uncertainty of each component and the extended uncertainty are calculated,the result of uncertainty is obtained.The results showed that when the florfenicol content of pork was 7.6μg·kg^(-1),the expanded uncertainty was 1.2μg·kg^(-1)(k=2),and when the florfenicol amine content was 7.0μg·kg^(-1),the expanded uncertainty was 1.1μg·kg^(-1)(k=2).The uncertainty of determination results mainly comes from the preparation process of mixed standard series working fluid.This study can provide an important reference for the process and result of determination of florfenicol and florfenicol amine in pork by GB 31658.5—2021.