超高效液相色谱-串联质谱法同时检测鸡蛋中5种磺胺类药物和甲氧苄啶残留量

Simultaneous Determination of Five Sulfonamide and Trimethoprim Residues in Eggs by Ultrahigh-performance Liquid Chromatography-tandem Mass Spectrometry

建立超高效液相色谱-串联质谱法(Ultrahigh-performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定鸡蛋中5种磺胺类药物(磺胺甲恶唑、磺胺二甲嘧啶、磺胺间甲氧嘧啶、磺胺喹噁啉、磺胺二甲氧嘧啶)和甲氧苄啶的残留量的方法。样品经乙腈提取2次,95%乙腈溶液进行溶解后,过Alumina B Cartridges柱,30%乙腈洗脱,滤膜过滤后滤液用于超高效液相色谱-串联质谱仪测定,外标基质标准曲线法定量。在0.5~100μg/kg的浓度范围内5种磺胺类药物和甲氧苄啶色谱峰面积与浓度呈良好线性相关,相关系数均大于0.99;方法检测限0.5μg/kg、定量限为1.0μg/kg;鸡蛋样品中5种磺胺类药物和甲氧苄啶在1.0~100.0μg/kg添加水平内的平均回收率在66.3%~97.5%之间,批内、批间相对标准偏差在1.4%~11.4%之间。该方法回收率满足残留检测要求,且方法的重现性良好,满足国内外兽药残留相关法规规定。

To establish a method for simultaneous determination of five kinds of sulfonamide(sulfamethoxazole,sulfamethazine,sulfamonomethoxine,sulfaquinoxaline,sulfadoxine)and trimethoprim residues in eggs by ultrahigh performance liquid chromatography-tandem mass spectrometry,samples were extracted twice with acetonitrile,dissolved in 95%acetonitrile solution,eluted with 30%acetonitrile on alumina b cartridges column,filtered with membrane,and determined by ultra high-performance liquid chromatography mass spectrometer.In the concentration range of 0.5~100μg/kg,the peak areas of five sulfonamide and trimethoprim showed a good linear correlation with the concentration,and the correlation coefficients were all higher than 0.99.The detection limit of the method was 0.5μg/kg and the quantitative limit was 1.0μg/kg.The average recoveries of five sulfonamide and trimethoprim in egg samples were between 66.3%and 97.5%at the addition level of 1.0~100.0μg/kg,and the relative standard deviation between batches was between 1.4%and 11.4%.The recovery rate of this method meets the requirements for residue detection,and this method has good reproducibility,which meets the relevant domestic and foreign veterinary drug residue regulations.