TurboFlow在线净化-液相色谱-串联质谱法测定畜禽肉中20种(氟)喹诺酮类兽药残留量  

Determination of 20(Fluoro) Quinolones Residues in Livestock and Poultry Meat by TurboFlow Online Cleanup-Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王炳玲[1] 田霁昕 项佳林[1] 艾连峰[1] WANG Bingling;TIAN Jixin;XIANG Jialin;AI Lianfeng(Hebei Entry-Exit Inspection and Quarantine Bureau,Shijiazhuang 050051,China;College of Food Science and Engineering,Shandong Agricultural University,Tai＇ an 271018,China)

机构地区：[1]河北出入境检验检疫局,河北石家庄050051 [2]山东农业大学食品科学与工程学院,山东泰安271018

出　　处：《肉类研究》2018年第5期30-38,共9页Meat Research

基　　金：国家质量监督检验检疫总局科技计划项目(2013IK154;2014IK092)

摘　　要：建立TurboFlow在线净化-液相色谱-串联质谱测定畜禽肉中20种(氟)喹诺酮类药物((Fluoro)quinolones,(F)QNs)残留量的分析方法。样品用甲醇-乙腈(1∶1,V/V)进行均质提取,Cyclone-p在线净化柱净化富集提取液中的(F)QNs,然后将富集所得分析物洗脱,转至Hypersil Gold C_8分析柱,经色谱分离后,用串联质谱检测。结果表明:西诺沙星、伊诺沙星和丹诺沙星在0.2～20.0 ng/mL的线性范围内线性良好,其余17种(F)QNs在0.1～10.0 ng/mL的线性范围内线性良好,且R^2均大于0.99;西诺沙星、伊诺沙星和丹诺沙星的定量限为2μg/kg,其余17种(F)QNs为1μg/kg;20种(F)QNs在3个水平的添加回收率为85.4%～108.2%,相对标准偏差为4.04%～8.57%。方法简单、快速、回收率高、重复性好,适用于动物源食品中(F)QNs的定量及确证检测。A new method was developed for the determination of（fluoro）quinolones（（F）QNs） residues in livestock and poultry meat using TurboFlow online cleanup（TFC）-liquid chromatography-tandem mass spectrometry（LC-MS/MS）. Samples were extracted with methanol-acetonitrile（1 ： 1, V/V） mixture. Then the extract was purified on a Cyclone-p column. Subsequently, the analytes were separated on a Hypersil Gold C8 column before being analyzed by tandem mass spectrometry. The calibration curves showed good linearity with R2 〉 0.99 in the concentration range from 0.2 to 20.0 ng/mL for cinoxacin, enrofloxacin and danofloxacin, and in the range from 0.1 to 10.0 ng/mL for 17 other（F）QNs. The limit of quantization for enrofloxacin, danofloxacin and cinoxacin was 2 μg/kg, while that for 17 other（F）QNs was 1 μg/kg. Average recoveries of the analytes fortified at three levels ranged from 85.4% to 108.2%, with relative standard deviations（RSDs） between 4.04% and 8.57%. The method was characterized by simplicity, rapidity, high recovery and good repeatability and was suitable for quantitative analysis and confirmation of（F）QNs residues in foods of animal origin.

关 键 词：TurboFlow在线净化液相色谱 串联质谱 (氟)喹诺酮类药物 残留 畜禽肉 

分 类 号：S859.84[农业科学—临床兽医学]