【摘要】 建立了非磺胺类兽药粉剂中磺胺二甲嘧啶、磺胺醋酰、磺胺甲噻二唑、磺胺氯哒嗪、磺胺甲基异唑、磺胺噻唑、磺胺-6-甲氧嘧啶、磺胺甲基嘧啶、磺胺邻二甲氧嘧啶、磺胺吡啶、磺胺对甲氧嘧啶、磺胺甲氧哒嗪、磺胺苯吡唑、磺胺间二甲氧嘧啶、磺胺二甲异唑、磺胺喹啉、磺胺嘧啶、甲氧苄氨嘧啶18种磺胺及其增效剂等违禁添加药物的超高效液相色谱-串联质谱分析方法。样品经甲醇-水(90∶10)萃取后,以乙腈(含0.1%甲酸)和水(含0.1%甲酸)为流动相,C18(2.1 mm×150 mm,5μm)色谱柱分离后,在正离子模式下以电喷雾串联质谱仪进行测定。方法的线性范围为50~2 000μg/kg,18种磺胺类药物残留的检出限为10μg/kg。在50,200,1 000μg/kg 3个浓度水平下进行加标回收实验,平均回收率为86.8%~115%,相对标准偏差为1.0%~9.7%。更多还原

【Abstract】 A high performance liquid chromatography-electrospray ionization triple-quadruple tandem mass spectrometric(HPLC-ESI-MS/MS) method was established for the determination of 18 sulfonamides and their potentiators in veterinary pharmaceutical powder, including sulfadimidine,sulfacetamide, sulfamethizole, sulfachloropyridazine, sulfamethoxazole, sulfathiazole, sulfamonomethoxine,sulfamerazine, sulfadoxine, sulfapyridine, sulfameter, sulfamethoxypyridazine, sulfaphenazolum, sulfadimethoxypyrimidine, sulfisoxazole, sulfaquinoxaline, sulfadiazine and trimethoprim. The 18 banned additives were extracted with methanol-H2O(90 ∶ 10). Then the reconstituted sample solution was analyzed by HPLC-MS/MS under positive ion mode,with a C18column(2. 1 mm × 150 mm,5 μm) as analytical column. The detection limits of 18 sulfonamides were all10 μg/kg. The calibration curves were linear in the range of 50-2 000 μg/kg,with correlation coefficients more than 0. 99. The method was validated at spiked levels of 50,200,1 000 μg/kg,and the overall recoveries were in the range of 86. 8%-115% with relative standard deviations(RSDs) of 1. 0%-9. 7%.更多还原