液相色谱-串联质谱法测定乳品中氟苯尼考和氟苯尼考胺残留量

Determination of Flufenicol and Flufenicol Amine Residues in Dairy Products by Liquid Chromatography-Tandem Mass Spectrometry

目的:建立液相色谱-串联质谱法测定乳品中氟苯尼考和氟苯尼考胺残留量的方法。方法:乳品试样用2%氨化乙酸乙酯溶液提取,经正己烷脱脂,再用2%氨化乙酸乙酯溶液反萃取,浓缩过膜后上机测试。结果:氟苯尼考和氟苯尼考胺在1~50μg·L^(-1)线性关系良好,检出限为0.5μg·kg^(-1),定量限为1μg·kg^(-1),加标回收率为82.5%~100.4%,RSD为3.35%~6.98%。结论:该方法适用于乳品中氟苯尼考和氟苯尼考胺残留量的定性、定量分析。

Objective:To establish a method for the determination of flufenicol and flufenicol amine residues in dairy products by liquid chromatography-tandem mass spectrometry.Method:Milk samples were extracted with 2%ethyl acetate solution,defatted with n-hexane,then back extracted with 2%ethyl acetate solution,concentrated and tested by machine.Result:The linear relationship between flufenicol and flufenicol amine was good in the range of 1~50μg·L^(-1).The limit of detection was 0.5μg·kg^(-1),the limit of quantitation was 1μg·kg^(-1),the recoveries were 82.5%to 100.4%,and the RSD was 3.35%to 6.98%.Conclusion:The method is suitable for the qualitative and quantitative analysis of flufenicol and flufenicol amide residues in dairy products.