高效液相色谱-串联质谱法测定兽药粉剂中18种磺胺类违禁添加药物  

Determination of 18 Sulfonamides in Veterinary Pharmaceutical Powder by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王晓利[1] 郭涛[2] 王珊珊[1] 赵金[1] 苑金鹏[1] 赵汝松[1] 

机构地区：[1]山东省科学院山东省分析测试中心,山东济南250014 [2]山东省农业科学院山东省水稻研究所,山东济南250010

出　　处：《分析测试学报》2015年第1期115-119,共5页Journal of Instrumental Analysis

基　　金：山东省自然科学基金项目(ZR2013BL011)

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%。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 C18 column（2.1 mm×150 mm,5 μm） as analytical column.The detection limits of 18 sulfonamides were all 10 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%.

关 键 词：磺胺类 高效液相色谱-串联质谱 兽药粉剂 

分 类 号：O657.72[理学—分析化学] TQ460.72[理学—化学]