高效液相色谱-串联质谱同位素内标法测定畜禽肉中地塞米松残留量

Determination of Dexamethasone Residue in Livestock and Poultry Meat by Isotope Internal Standard Method with High Performance Liquid Chromatography-Tandem Mass Spectrometry

目的:开发一种基于高效液相色谱-串联质谱的分析方法,用于快速测定畜禽肉中的地塞米松残留量。方法:样品经0.2%甲酸乙腈提取,ECS亲水亲脂萃取柱净化后,用高效液相色谱-串联质谱仪测定,同位素内标法进行定量分析。结果:地塞米松在0.5~100.0 ng·mL^(-1)范围内呈现良好线性关系,相关系数R> 0.999,方法定量限为0.2μg·kg^(-1);空白样品在0.5μg·kg^(-1)、2.5μg·kg^(-1)和10.0μg·kg^(-1)添加水平时,平均回收率为92.2%~99.6%,相对标准偏差为0.6%~2.5%(n=6),方法学指标均满足《实验室质量控制规范食品理化检测》(GB/T 27404—2008)要求。结论:本研究建立的方法具有操作简单、准确度高、重复性好等特点,适用于畜禽肉中地塞米松残留量的测定。

Objective:To develop an analytical method based on high performance liquid chromatography-tandem mass spectrometry for the determination of dexamethasone residues in meat from livestock and poultry.Method:The samples were extracted by 0.2% acetonitrile,purified by ECS hydrolipophilic extraction column,determined by high performance liquid chromatography-tandem mass spectrometry,and quantitatively analyzed by isotope internal standard method.Result:The linear relationship of dexamethasone was good in the range of 0.5~ 100.0 ng·mL~(-1) with correlation coefficient more than 0.999,and the limit of quantification was 0.2 μg·kg^(-1).At the spiked levels of 0.5 μg·kg^(-1),2.5 μg·kg^(-1) and 10.0 μg·kg^(-1),the average recovery was from 92.2% to 99.6%,the relative standard deviation was from 0.6% to 2.5%(n=6).All the methodological indicators meet the technical requirements of GB/T 27404—2008.Conclusion:The method established in this study has the characteristics of simple operation,high accuracy and good repeatability,and is suitable for the determination of dexamethasone residue in livestock and poultry meat.