论文部分内容阅读
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。
OBJECTIVE: To establish a rapid solid phase extraction coupled with ultra performance liquid chromatography (UPLC) tandem mass spectrometry for rapid determination of 11 common sulfonamides (sulfonamides, sulfathiazole, sulfapyridine, sulfamerazine, sulfadoxine, sulfamethizole, Methoxypyrimidine, sulfamethoxazole, sulfamethazine, sulfamethazine and sulfamethoxazole.Methods: After the protein was precipitated by acetonitrile and purified by Waters oasis MCX solid phase extraction cartridge, Tandem quadrupole electrospray ionization positive ion scan, multiple reaction monitoring (MRM) mode detection using a Waters Acquity BEHC18 column (1.7 μm, 2.1 mm × 50 mm) with 0.2% aqueous acetic acid: acetonitrile = 80:20 Phase at a flow rate of 0.3 ml / min and a column temperature of 40 ° C.Results: The quantitative detection limit of 11 sulfonamides residues in the range of 5μg / L ~ 200μg / L was 0.03μg / kg ~ 0.20μg / kg, Can reach 68.3% -108% with relative standard deviation of less than 10% .Conclusion: The method is simple, accurate, rapid and sensitive to meet the international minimum residue requirements for sulfonamides.