高效液相色谱-串联质谱法同时测定动物源性食品中24种磺胺类药物残留  

Simultaneous determination of 24 sulfonamides residues in animal products by high performance liquid chromatography tandem mass spectrometry

作　　者：刘佳佳[1] 佘永新[1] 刘洪斌[1] 王静[1] 吕晓玲[1] 王淼[1] 史晓梅[1] 徐思远[1] 肖航[1] 

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所中国农业科学院农产品安全重点实验室,北京100081

出　　处：《分析试验室》2011年第2期9-13,共5页Chinese Journal of Analysis Laboratory

基　　金："十一五"国家科技支撑计划项目(2006BAD12B03-06);国际先进农产品质量安全控制技术引进与示范项目(G2006)资助

摘　　要：利用高效液相色谱-电喷雾串联四极杆质谱(HPLC-MS/MS)联用技术,建立了一种在28 min内快速分离和测定鸡肉、猪肉、牛肉、羊肉、蜂蜜、牛奶中24种磺胺类药物残留的方法。方法检出限(LOD)为0.27～7.45μg/kg,定量限(LOQ)0.957～9.89μg/kg;在5～300μg/L范围内线性关系良好,在10、20、50μg/kg 3个添加浓度上回收率为60.8%～122.9%,相对标准偏差(RSD)为0.01%～19%。A selective and sensitive method has been residue levels of sulfonamides in chicken, pork, beef, developed and applied to the simultaneous determination of mutton, honey and bovine milk samples in 28 minutes using liquid chromatography tandem mass spectrometric （LC-MS/MS）. The sulfonamides were extracted with acetonitrile, followed by homogenizing, ultrasound treating and centrifuging. The extract was dried by rotary evaporator, redissolved in the initial mobile phase and defatted with n-hexane saturated by acetonitrile（except the honey）. The chromatographic analysis was performed on a Agilent Eclipse XDB-C18 column （2. 1 × 150 mm, 5 μm）using a gradient elution program of 0. 2% acetic acid and acetonitrile as a mobile phase. The flow rate is 0. 2 mL/min. Using LC-MS/MS （ESI） with multiple reaction monitoring （MRM）, identification of the major components of 24 sulfonamides were performed based upon the intensities of mass fragments. Recoveries of 24 sulfonamides at the spiked Concentration levels of 10μg/kg, 20μg/kg and 50μg/kg ranged from 60. 8% to 122.9% with RSD, were 0.01% - 19%, The calibration curves showed good linearity in the range of 5 -300 μg/L for all sulfonamides with detection limits of 0. 27 -7.45μg/kg and quantization limits of 0. 957 9.89 μg/kg. The testing results of different laboratories have no significant differences. The method is suitable for quantitative and qualitative analysis of sulfonamides in a variety of samples.

关 键 词：液相色谱-串联质谱 动物源性食品 磺胺 残留 检测 

分 类 号：O657.63[理学—分析化学]