液相色谱_串联质谱内标法同时测定水产品中15种喹酮类药物残留量

:20090723:20091230:863(No.2008AA100805);(Nyhyzx07046);(2007gy02)*:,,,.第26卷第4期Vol.26No.4分析科学学报JOURNALOFANALYTICALSCIENCE2010年8月Aug.2010:10066144(2010)0404090615王志杰,冷凯良*,孙伟红,宁劲松,翟毓秀,谭志军,郭萌萌(,266071):建立了水产品中15种喹诺酮类药物(QNs)残留量的高效液相色谱串联质谱(HPLCMS/MS)测定方法以氘代试剂为内标,样品经酸性乙腈萃取后,用正己烷脱脂,旋转蒸发浓缩,采用HPLCMS/MS选择反应监测(SRM)正离子模式测定,内标法定量可同时对水产品中的15种QNs进行定性和定量测定15种QNs的检出限(S/N=3)为1.0g/kg,定量限(S/N=10)为2.0g/kg;在10.0~200.0ng/mL时峰强度与质量浓度的线性关系良好(r0.99)方法的平均回收率范围为66%~121%该法简便快捷,分析成本低,在一定程度上实现了药物残留的快速检测:高效液相色谱串联质谱;内标法;水产品;喹诺酮类药物;多残留同时测定:O657.63:A(Quinolones,QNs)80,,,,QNs,,QNsQNs,QNs,,(MRL),QNs[13][48],(HPLCMS/MS),QNs,,QNs3QNs,HPLCMS/MS15QNs,,,,,,11.1ThermoFinniganTSQQuantumAccess,ESI,,,409第4期王志杰等:高效液相色谱串联质谱内标法同时测定水产品中15种喹酮类药物残留量第26卷QNsWitega(99.5%):QNs,(,),1.0mg/mL,-18,6:QNs,,1.0g/mL0.1g/mL,4,1:,(),0.5mg/mL,-18,6:,,1.0g/mL,4,1;;0.1%(5.0mmol/L);:99mL1mLGB/T66821.21.2.1C18(MG!,150∀2.1mm,5m)();:10L;:A0.1%(5.0mmol/L),B,C11Table1TheconditionofgradientelutionTime(min)Flowrate(L/min)ABC0200782023.0200752056.02007020108.02004020401320040204013.12007820216200782021.2.2:(ESI),;:4500V;:12L/min;:2L/min;:350;:6V;:(SRM),2;Q1:0.7Da;Q3:0.7Da;:,1.5mTorr15QNs2215QNsTable2ESIMS/MSconditionsfor15QNsAnalyteParention(m/z)Daughterion(m/z)Collisionenergy(eV)AnalyteParention(m/z)Daughterion(m/z)Collisionenergy(eV)Fleroxacin37026926Difloxacin40029928326*19356*19Ofloxacin36226127Sarafloxacin38629926318*18342*18Norfloxacin32023324Sparfloxacin39329225276*16349*19Enoxacin32123234Oxolinicacid26221629303*21244*18Ciprofloxacin33224522Flumequin26220232288*17244*18Enrofloxacin36024526Pefloxacin33429018316*9316*20Lomefloxacin35226522NorfloxacinD5325307*22308*16Danofloxacin35828322CiprofloxacinD8340322*21340*22Orbifloxacin39629524EnrofloxacinD5365321*19352*17*Representthemostabundantions.410第4期分析科学学报第26卷1.35.0g50mL,50L,30s,10min10.0g,,20mL,1min,10min,4000r/min5min,50mL,,401.0mL(#=20#80,V/V),2.0mL30s,5mL,4000r/min5min,,0.2m,2.12.1.1QNs,C8C18QNs,50%,EclipsXDBC18HypurityC18MG!C18,:XDBC18,HypurityC18QNs,,,MG!C18QNs,MG!C18,2.1.215QNs,,,,,,,,,,,,15QNs0.1%pH(pH=2~3),,,QNs,,,,12115QNsFig.1Chromatogramsof15QNsandinternalstandardspikedinashrimpsampleSpikedlevel:5.0g/kg.411第4期王志杰等:高效液相色谱串联质谱内标法同时测定水产品中15种喹酮类药物残留量第26卷215QNsFig.2Chromatogramsof15QNsandinternalstandardspikedinaneelsampleSpikedlevel:5.0g/kg.2.220L/min2g/mL15QNs,m/z200~450,[M+1]+,QNs,,,,[M+HH2O][M+HCO2][M+HCH3N=CH2],,(SRM)(SkimmerOffset)(CollisionEnergy)2.32.3.1QNs()(),;,,,pH3,,,1%,,,()QNs,,,,5g10g,2.3.2,,,2.3.3(#=50#50)(#=20#80),HPLCMS/MS:,#(50#50,V/V);(#=20#80)(#=20#80)(#=20#80),,,412第4期分析科学学报第26卷2.410.0~200.0ng/mL,,,,15QNs,0.99,1.0g/kg15QNs,(S/N)3,15QNs1.0g/kg2.0g/kg,15QNs(S/N)10,2.0g/kg2.5,15QNs,6,3,,∃12.9%,∃17.8%15QNs312315QNs(n=6)Table3Recoveriesof15QNsfromspikedeelandshrimp(n=6)AnalyteAdded(g/kg)Averagerecoveryfromeel(%)RSD(%)Averagerecoveryfromshrimp(%)RSD(%)AnalyteAdded(g/kg)Averagerecoveryfromeel(%)RSD(%)Averagerecoveryfromshrimp(%)RSD(%)2.073.211.275.110.62.068.514.869.112.4Fleroxacin5.093.38.985.55.4Orbifloxacin5.071.911.779.29.310.090.64.289.72.710.075.38.778.67.92.0118.413.2112.410.42.081.814.677.211.9Ofloxacin5.0116.19.7115.97.6Difloxacin5.078.912.884.87.710.0109.27.5106.16.510.090.88.392.85.82.077.89.975.48.22.066.815.074.113.9Norfloxacin5.090.39.482.25.6Sarafloxacin5.073.312.176.812.510.086.45.594.64.610.077.19.475.28.72.081.59.878.47.92.0108.314.495.612.9Enoxacin5.079.17.486.65.8Sparfloxacin5.097.613.691.010.310.089.34.892.42.910.0102.210.9108.16.72.080.09.678.38.72.083.411.0111.89.7Ciprofloxacin5.088.97.186.95.3Oxolinicacid5.081.47.198.98.310.094.23.896.52.310.090.94.4103.55.02.0110.38.8105.97.62.078.19.875.58.8Enrofloxacin5.0106.76.4108.35.7Flumequin5.074.23.480.67.610.095.93.4100.54.110.084.94.282.73.92.072.714.376.911.42.070.89.1112.48.9Lomefloxacin5.076.510.981.88.4Pefloxacin5.086.16.498.77.110.083.87.889.74.910.093.74.6104.62.82.0120.613.3109.512.4Danofloxacin5.0116.510.7107.49.110.0105.47.398.78.62.615,,1.2g/kg,,QNs315QNsHPLCMS/MS,QNs,15QNs,,413第4期王志杰等:高效液相色谱串联质谱内标法同时测定水产品中15种喹酮类药物残留量第26卷:[1]WANGHongyan(),LIZhaoxin(),LINHong().MarinFisheriesResearch()[J],2007,28(3):80.[2]DONGLinlin(),LIUYanhua(),WANGXia().ChineseJournalofChromatography()[J],2005,23(3):285.[3]DULiming(),WEIHongqing(),ZHANGJunyan().ChineseJournalofChromatography()[J],2003,21(5):503.[4]FuhMS,ChanSA,WangHL.Talanta[J],2000,(52):141.[5]SHIBing(),ZHANGZhigang(),WUShuhua().InspectionandQuarantineScience()[J],2004,14():26.[6]CHENXiaohong(),YAOXunping().ChinsesJournalofHealthLaboratoryTechnology()[J],2007,17(9):1572.[7]PENGTao(),YONGWei(),ANJuan().ChineseJournalofAnalyticalChemistry()[J],2006,(34):10.[8]FuhMS,ChanSA,WangHL.Talanta[J],2000,(52):141.SimultaneousDeterminationof15QuinoloneResiduesinAquaticProductsbyHPLCMS/MSwithInternalStandardMethodWANGZhijie,LENGKailiang*,SUNWeihong,NINGJinsong,ZHAIYuxiu,TANZhijun,GUOMengmeng(YellowSeaFisheriesResearchInstitute,ChineseAcademyofFisherySciences,Qingdao266071)Abstract:Amethodforsimultaneousdeterminationof15QNsresiduesinaquaticproductswasdevelopedbyhighperformanceliquidchromatographytandemmassspect