高效液相色谱-电喷雾串联质谱法测定水产品中14种喹诺酮类与磺胺类药物残留

建立了高效液相色谱-电喷雾串联质谱法测定水产品中恩诺沙星、环丙沙星、双氟沙星、沙拉沙星、氟甲喹、喹酸、磺胺嘧啶、磺胺甲唑、磺胺喹啉、磺胺甲基嘧啶、磺胺二甲氧嘧啶、磺胺二甲基嘧啶、磺胺间二甲氧嘧啶、甲氧苄胺嘧啶共14种常用喹诺酮类与磺胺类兽药的残留检测方法。样品制备后,采用1%乙酸-乙腈提取液提取,用正己烷净化处理后,采用LC/MS/MS电喷雾电离(ESI),多反应监测(MRM)正离子模式检测,外标法定量。在0～100μg/kg范围内14种兽药的线性相关系数均>0.99。在添加浓度5～50μg/kg范围内,14种药物的回收率在70.0%～110%,相对标准偏差(RSD)均在12%以内。方法的检出限为0.1～0.5μg/kg。

Determination of 14 quinolones and sulfonamides medicine residuces in aquatic product using high performance liquid chromatography-electrospray ionization tandemmass spectrometry

A method for the determination of 14 quinolones and sulfonamides medicine resisduces,enrofloxacin,ciprofloxacin,sarafloxacin,difloxacin,flumequine,oxilinic acid,sulfamethoxazole,sulfadiazine,sulfaquinoxaline,sulfamerazine,sulfamethazine,sulfamonomethoxine,sulfadimethoxine,trimethoprim in aquatic product was developed by using high performance liquid chromatography-electrospray ionization tandem mass spectrometry(HPLC-ESI MS/MS).After homogenization,samples were extracted with 1% acetic acid-acetonitrile.The extracts were cleaned by hexyl hydride.Identification and detection were achieved by electrospray ionization(ESI) in positive mode using multiple reaction monitoring of liquid chromatography coupled with tandem mass spectrometry.The linearity of all the 14 quinolones and sulfonamides medicine in the range from 0 to 100 μg/kg is correlation coefficient greater than 0.99.Antibiotics are quantified by external standard method.Recoveries are within 70.0%~110.0% at the spiked level of 5 to 50 μg/kg.The relative standard deviations(RSDs) for the 14 quinolones and sulfonamides medicine are less than 12%.The detection limits were 0.1 to 0.5 μg/kg.