电喷雾超高效液质联用法测定动物性食品中磺胺类药残

目的:建立固相萃取-超高效液相色谱(UPLC)串联质谱法快速测定11种常用磺胺类化合物(磺胺、磺胺噻唑、磺胺吡啶、磺胺甲基嘧啶、磺胺多辛、磺胺甲二唑、磺胺间甲氧嘧啶、磺胺氯达嗪、磺胺二甲异恶唑、磺胺二甲氧嘧啶、磺胺喹恶啉的方法。方法:加入乙腈沉淀蛋白后经Waters oasis MCX固相萃取小柱净化后,使用串联四极杆电喷雾离子源正离子扫描,多反应监测(MRM)模式检测,采用Waters Acquity BEHC18分离柱(1.7μm,2.1 mm×50 mm),0.2%乙酸水溶液∶乙腈=80∶20为流动相,流速0.3 ml/min,柱温为40℃。结果:在5μg/L～200μg/L的线性范围内11种磺胺药残的定量检测下限为0.03μg/kg～0.20μg/kg,回收率能达到68.3%～108%,相对标准偏差小于10%。结论:本方法操作简单、准确、快速,灵敏度满足国际上对磺胺类药物的最低残留限量要求。

Determination of 11 kinds of sulfonamides in animal foods by ESI-UPLC-MS/MS

Objective:To creat a mehod for rapid determination of 11 sulfonamides(sulfanilamide,sulfathiazole,sulfapyridine,sulfamerazine,sulfadoxine,sulfamethizol,sulfamonomethoxine,sulfachloropyridazine,sulfisoxazole,sulfadimethoxine,sulfachinoxaline) in animal foods by SPE-ultra performance liquid chromatography(UPLC) with MS/MS detector.Methods: After extracted by acetonitrile,purified through Waters oasis MCX SPE column,the sulfonamides were detected by UPLC-MS/MS ESI(+) MRM mode.The mobile phase was a mixture of 0.2% acetic acid and acetonitrile(80∶ 20),the flow rate was 0.3 ml/min,Waters Acquity BEH C18(1.7 μm,2.1 mm×50 mm) was separation column,the column temperature was 40℃.Results: The detection limits of 11 kinds of sulfonamides in animal foods were between 0.03 μg/kg~0.20 μg/kg,the recoveries were between 68.3%~108%,the relative standard deviations were less than 10%.Conclusion: The method with the advantages of simpleness,accuracy,speediness and sensitivity can meet the international minimum residue limit detection of sulfonamides.