QuEChERS-高效液相色谱-质谱法测定禽、畜肉中氨基比林

QuEChERS-High Performance Liquid Chromatography Tandem Mass Spectrometry-Determination of Aminopyrine in Poultry and Livestock Meat by Mass Spectrometry

建立QuEChERS-高效液相色谱-质谱法测定禽、畜肉中氨基比林残留量的分析方法。液相色谱条件为:色谱柱C18( 2.1×50mm,1.8μm);流动相为A:5mmol/L乙酸铵+0.1%甲酸水溶液,B:乙腈;梯度洗脱;柱温为35℃;流速为0.2mL/min;进样量为2μL。质谱条件为:电喷雾离子源(ESI+),多反应监测(M RM)方式进行采集。结果表明:优化的最佳QuEChERS组成为:4gNa2SO4、1gNaCl作为萃取盐,乙腈(1%乙酸)作为萃取溶剂,d-SPE过程中使用600mgNa2SO4、150mgC18,方法的最低定量限为0.1μg/kg,氨基比林在0.02~10μg/L范围内有良好的线性关系,在0.5~5.0μg/kg的浓度添加水平上,其回收率在89.3%~102.2%,相对标准偏差小于15%。改进的QuEChERS方法前处理便捷,灵敏度高,回收率高,适用于禽、畜肉中氨基比林残留量的测定。

To establish the method of QuEChERS- high performance liquid chromatography-mass spectrometry for the de termination of ampicillin residues in poultry and livestock meat. The liquid chromatography conditions are:chromatograph ic column C18( 2.1×50mm,1.8μm);the mobile phase is:A:5mmol/L ammonium acetate+0.1% aqueous formic acid,B: acetonitrile;gradient elute;column temperature is 35℃;the flow velocity is 0.2mL/min;the sample size is 2μL. The mass spectrometry conditions are:Electrospray ionization Source( ESI+),multi-response monitoring( MRM) is used for collec tion. The results show:The optimized composition of QuEChERS is:4g Na2SO4 and 1gNaCl are used as extraction of salt, acetonitrile( 1% acetic acid)is used as extracting solvent,600mg Na2SO4 and 150mg C18 are used in the d-SPE process. The minimum quantitative limit of the method is 0.1μg/kg,there is a good linear relation when the aminopyrine is wihtin 0.02~10μg/L,for the level of 0.5~5.0μg/kg concentration,the recovery rate is 89.3%~102.2%,the relative standard de viation is less than 15%. The improved QuEChERS method has advantages of convenient pretreatment,high sensitivity and high recovery,which is suitable for the determination of aminobilin residues in poultry and livestock meat.