牛奶中16种喹诺酮类药物残留量的高效液相色谱-串联质谱法测定  

Determination of 16 Quinolones Residues in Milk by High Performance Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

作　　者：岳振峰[1] 谢丽琪[1] 陈小霞[2] 吉彩霓[1] 林秀云[1] 侯乐锡[1] 欧阳姗[1] 

机构地区：[1]深圳出入境检验检疫局食品检验检疫技术中心,广东深圳518067 [2]深圳大学教务处,广东深圳518060

出　　处：《分析测试学报》2008年第3期240-243,共4页Journal of Instrumental Analysis

摘　　要：建立了牛奶样品中萘啶酸、嗯喹酸、氟甲喹、诺氟沙星、依诺沙星、环丙沙星、洛美沙星、丹诺沙星、恩诺沙星、氧氟沙星、沙拉沙星、二氟沙星、麻保沙星、培氟沙星、司帕沙星、奥比沙星16种喹诺酮类兽药多残留量的液质联用确证方法。用酸性乙腈萃取样品中16种喹诺酮类药物残留，然后用正己烷脱脂，旋转蒸发仪浓缩，以Inertsil C8-3色谱柱为分离柱，在正离子模式下以电喷雾电离串联质谱仪进行测定。在10、50、100μg/kg 3个浓度水平进行验证实验，方法的线性范围为10-100μg／kg，平均回收率为69％-104％，相对标准偏差为4.1％-12.7％。A confirmative method was developed with high-performance liquid chromatography tandem electrospray mass spectrometry（ LC- MS/MS） to simultaneously determine 16 residues of quinolones in milk, including nalidixinic acid, oxolinic acid, flumequine, norfloxacin, enoxacin, ciprofloxacin, lomefloxacin, danofloxacin, enrofloxacin, ofloxacin, sarafloxacin, difloxacin, marbofloxacin, pefloxacin, sparfloxacin and orbifloxacin. 16 residues were extracted with acidified acetonitrile, cleaned with hexane, and concentrated with rotal3, evaporator. Then the reconstituted sample solution was analyzed by LC - MS/MS under positive ion mode, with Inertsil C8-3 column as the analytical column. The method was validated at 10, 50 and 100μg/kg, with the linear range from 10μg/kg to 100μg/kg; the overall recovery, from 69% to 104% , and the relative standard deviation（RSD） between 4.1% and 12.7% .

关 键 词：喹诺酮类 残留 液相色谱 串联质谱 牛奶 

分 类 号：O657.63[理学—分析化学] TQ455.5[理学—化学]