液相色谱-串联质谱法测定常见食品中磺胺及喹诺酮  

Determination of Sulfonamides and Quinolones in Common Foods with Liquid Chromatographic-tandem Mass Spectrometry

作　　者：于维森[1] 于红卫[1] 郝文[1] 吕晓静[1] 

机构地区：[1]青岛市疾病预防控制中心,山东青岛266033

出　　处：《预防医学论坛》2011年第2期102-105,共4页Preventive Medicine Tribune

基　　金：国家"十一五"科技支撑计划项目--重大活动中食品安全保障技术研究与示范(2006BAK02A27);青岛市科技局立项课题(06-3-2-2NSH)

摘　　要：[目的]本试验研究建立常见17种磺胺和15种喹诺酮类药物残留量的液相色谱-电喷雾串联离子阱质谱测定方法。[方法]以稳定同位素氘代磺胺邻二甲氧嘧啶、氘代磺胺间二甲氧嘧啶作为内标,采用多反应监测定量。样品经过匀浆、超声波提取、甲醇溶液涡旋溶解残留物、正己烷涡旋混合离心后进行液相色谱-质谱分析。采用C18柱,MGⅡ色谱柱,以均含0.1%甲酸的水和甲醇、乙腈为流动相进行梯度洗脱。[结果]17种磺胺和15种喹诺酮类药物的线性范围为2.0~50μg/kg,相关系数r〉0.995,平均回收率为83.3%~109.9%（添加水平为2.5~10μg/kg）,相对标准偏差为2.1%~8.1%。本方法最低检出限均为2.0μg/kg,最低定量限均为4.0μg/kg。[结论]所建方法简便、快速、干扰少、特异性强,是磺胺和喹喏酮残留检测的理想方法。[Objective]This experiment research was to establish a liquid chromatographic-electrospray ionization tandem mass spectrometry method ion trap for determining common 17 kinds of sulfonamides and 15 kinds of quinolones residue.[Methods]Take stable isotopes deuterium sulfonamides adjacent dimethyl oxygen pyrimidine,deuterium between dimethyl oxygen pyrimidine sulfonamides as internal standard,and the reaction monitoring as quantitative method.Sample after homogenate,ultrasonic extraction,methanol solution vortex dissolve residues were hexane vortex mixed centrifugal after liquid chromatography-mass spectrum analysis.Using C18 column,MG Ⅱ chromatographic column to all contain 0.1% formic acid water and methanol,acetonitrile as mobile phase for gradient elution.[Results]The linear range for 17 kinds of sulfonamides and 15 kinds of quinolone was 2.0-50 μg/kg,correlation coefficient R was0.995,and the average recovery was 83.3%-109.9%（added level for 2.5-10 μg/kg）,relative standard deviation was 2.1%-8.1%.The minimum detection limit of the method was 2.0 μg/kg,minimum loq was 4.0 μg/kg.[Conclusion]The method established was simple,rapid,less disturbance,strong specificity,it was the ideal method for sulfonamides and fluorine quinoline ahoy ketone residue detection.

关 键 词：食品 磺胺 喹诺酮 液相色谱-质谱分析 选择离子监测方式 

分 类 号：R155[医药卫生—营养与食品卫生学]