资源描述:
《turboflow在线净化-液相色谱-串联质谱法测定》由会员上传分享,免费在线阅读,更多相关内容在工程资料-天天文库。
1、302018,Vol.32,No.5肉类研究中国肉类食品综合研究中心分析检测MEATRESEARCHCHINAMEATRESEARCHCENTERTurboFlow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1211,*王炳玲,田霁昕,项佳林,艾连峰(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)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。
2、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HypersilGoldC8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0.2~20.0ng/mL的线性范围内线性良好,其余17种2(F)QNs在0.1~10.0ng/mL的线性范围内线性良好,且R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
3、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。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Determinationof20(Fluoro)QuinolonesResiduesinLivestockandPoultryMeatbyTurboFlowOnlineCleanup-LiquidChromatography-TandemMassSpectrometry1211,*WANGBingling,TIANJixin,XIANGJialin,A
4、ILianfeng(1.HebeiEntry-ExitInspectionandQuarantineBureau,Shijiazhuang050051,China;2.CollegeofFoodScienceandEngineering,ShandongAgriculturalUniversity,Tai’an271018,China)Abstract:Anewmethodwasdevelopedforthedeterminationof(fluoro)quinolones((F)QNs)residuesinlivestockandpoultrym
5、eatusingTurboFlowonlinecleanup(TFC)-liquidchromatography-tandemmassspectrometry(LC-MS/MS).Sampleswereextractedwithmethanol-acetonitrile(1:1,V/V)mixture.ThentheextractwaspurifiedonaCyclone-pcolumn.Subsequently,theanalyteswereseparatedonaHypersilGoldC8columnbeforebeinganalyzedby
6、tandem2massspectrometry.ThecalibrationcurvesshowedgoodlinearitywithR>0.99intheconcentrationrangefrom0.2to20.0ng/mLforcinoxacin,enrofloxacinanddanofloxacin,andintherangefrom0.1to10.0ng/mLfor17other(F)QNs.Thelimitofquantizationforenrofloxacin,danofloxacinandcinoxacinwas2μg/kg,wh
7、ilethatfor17other(F)QNswas1μg/kg.Averagerecoveriesoftheanalytesfortifiedatthreelevelsrangedfrom85.4%to108.2%,withrelativestandarddeviations(RSDs)between4.04%and8.57%.Themethodwascharacterizedbysimplicity,rapidity,highrecoveryandgoodrepeatabilityandwassuitableforquantitativeana
8、lysisandconfirmationof(F)QNsresiduesinfoodsofanimalorigin.Key