固相萃取_高效液相色谱_串联质谱同时检测动物源性食品中76种兽药残留

DOI10.3724/SP.J.1096.2010.00318-/761*111223120013522004333211198-/SPE-HPLC/MS76。Mg2+-95∶5V/V-。0.5μg/kgβ-、1.0μg/kg、5.0μg/kg20μg/kg。76、、、r0.90759.4%～115.3%2.6%～27.3%。20.926.5μg/kg。-2009-08-162009-10-25No.08DZ0505200No.HK004-2007*[e-mail]120。、1。β-2、3、4、56。7～9。-。101170～100。-/、、、676。。22.1API4000ABUFLCXRThermoAquasilC18150mm×4.6mm3.5μmAllegraX-22RBeckmanSuplcoBuchiN-EVAP111Organomatian-60mg3mL60mg3mLCNW0.5～10μL20～200μL200～1000μL3820103FENXIHUAXUEChineseJournalofAnalyticalChemistry3318～324500～5000μLBrand0.45μmΦ25mm0.22μLΦ13mmMillipore。HPLCJ.T.BakerHPLCPromptarHPLCPromptarACSJ.T.Baker、、、C6H8O7·H2O、MgCl2·6H2OACSFisher。β-12、14、10、192≥95%1.0g/L19。pH=2.510.5gC6H8O7·H2O10.2gMgCl2·H2O450mLpH2.5500mL。2.2/30℃0.6mL/min20μLA0.1%B0.1%95∶50～3min0～25%A3～4min25%～40%A4～7min40%～50%A7～9min50%A9～13min50%～100%A13～18.5min100%A18.5～23min100%B。ESI+GS10.448MPa550℃CUR0.207MPaGS20.483MPaIS4500VCE、DP1http//。EP10VCXP13Vβ-20ms、、、5ms。176Table1Multiplereactionmonitoringtransitionandmassspectrometryparametersofrepresentativecompoundswithin76veteri-narydrugsbrieftableCompoundCASNo.MolecularformulaPrecusorionm/zProductionm/zCollisionvoltageVDeclusteringpotentialVBenzodiazepine19Diazepam439-14-5C16H13ClN2O285.2193.2154.2*37388084Chlordiazepoxide58-25-3C16H14ClN3O300.2227.2282.2*32334266Alprazolam28981-97-7C17H13ClN4309.1274.3*205.1373410098α-α-Hydroxyalprazolam37115-43-8C17H13ClN4O325.1297.2*176.134388490Sulfonamide19Sulfaquinoxaline59-40-5C14H12N4O2S301.1156.0*108.0233910898Sulfadiazine68-35-9C10H10N4O2S251.192.1156.0*41236470Sulfamethoxypyridazine80-35-3C11H12N4O3S281.1156.0*215.024256070Benzimidazole14Albendazole54965-21-8C12H15N3O2S266.2234.2*191.230488888Febantelpestanal58306-30-2C20H22N4O6S447.3383.2*280.227449090Oxfendazole53716-50-0C15H13N3O3S316.2191.2*159.23148100100β-β-agonist12Ractopamine97825-25-7C18H23NO3302.2164.2*107.124516666Salbutamol18559-94-9C13H21NO3240.2148.2*27166666Clenbuterol37148-27-9C12H18Cl2N2O277.1203.1*132.1254275759133-/761ContinuedtoTable1CompoundCASNo.MolecularformulaPrecusorionm/zProductionm/zCollisionvoltageVDeclusteringpotentialVTriphenylmethane2LeucomalachiteGreen129-73-7C23H26N2331.2239.2*315.23937104113LeucocrystalViolet603-48-5C25H31N3374.3358.4*238.33935104110Nitroimidazole10Metronidazole443-48-1C6H9N3O3172.0128.2*82.121355551Dimetridazole551-92-8C5H7N3O2142.096.0*81.023366059Ronidazole7681-76-7C6H8N4O4201.1140.2*110.217253738*Quantitativetransition。2.32.3.15g50mL30mL、2mL10mL2000r/min5min4000r/min5min250mL。6mL40℃5mL50mL5mL4℃8500r/min10min0.45μm。2.3.23mL、3mL3mL。0.5mL/min。3mL、3mL、3mL-5∶95V/V5min4mL6mL-95∶5V/V40℃。1.0mL0.1%-9∶1V/V0.22μm。33.13.1.1。76、。pKa。pKa2.8～11.4。、、0.1mol/LpH=2.5Mg2+12。MgCl2-。3.1.2。。pH=2.5。76。1%3%5%10%-5%-。。023383.23.2.13ThermoAquasilC18150mm×4.6mmi.d.3.0μm、SunfireC18150mm×2.1mmi.d.3.0μmXbridgeC8150mm×2.1mmi.d.5.0μm762.05.010mmol/L0.1%、0.1%-、0.1%-。ThermoAquasilC18150mm×4.6mmi.d.3.0μm、。5%、、-6-281/156311/156215/1565--298/2661。1Fig.1MRMchromatogramofcompoundswithidenticalprecursorandproductions3.2.2CACEU657/2002/EEC13MRM。、。MRM。Dwelltimeβ-20ms、、、5ms1。3.33.3.1LOQ、、、。10S/N10760.1～0.5μg/kgβ-、0.2～0.5μg/kg、0.2～1.0μg/kg、0.5～1.0μg/kg、1.0～5.0μg/kg5.0～20.0μg/kg、2。3.3.2-14。、、、0.5～10.0μg/Lβ-2.0～50.0μg/L10.0～200.0μg/L5.0～50.0μg/L。3。1233-/762、、、5、Table2LOQrangeofrecoveryrelativestandarddeviationlinearcorrelationcoefficientofrepresentativecompoundswithin76veterinarydrugsinspikedsamplematrixregardingshrimpporklivermilkandeggBrieftableCompoundLOQμg/kgSpikedμg/kgRecovery%RSD%n=6rBenzodiazepineDiazepam0.21.02.04.075.0～92.13.0～10.80.963～0.999Chlordiazepoxide1.01.02.04.074.7～94.53.4～8.20.946～0.992Alprazolam0.21.02.04.068.5～94.04.6～10.60.997～0.999α-α-Hydroxyalprazolam0.51.02.04.069.7～94.63.3～8.30.984～1.000SulfonamideSulfaquinoxaline20.020.040.080.067.8～91.22.9～7.90.9929～0.9999Sulfadiazine5.020.040.080.069.6～91.93.6～10.60.967～1.000Sulfamethoxypyridazine5.020.040.080.072.5～97.63.3～7.80.960～0.999BenzimidazoleAlbendazole1.05.010.020.063.1～94.75.2～9.60.915～0.997Febantelpestanal5.05.010.020.071.8～94.32.6～13.10.938～0.998Oxfendazole2.05.010.020.074.5～96.84.6～12.40.944～0.995β-β-AgonistRactopamine0.30.51.02.064.4～101.43.9～11.90.937～0.997Salbutamol0.20.51.02.065.9～107.95.1～20.80.910～0.999Clenbuterol0.10.51.02.066.7～100.44.5～12.70.938～0.997TriphenylmethaneLeucomalachiteGreen0.20.51.02.069.2～101.17.9～16.50.919～0.984LeucocrystalViolet0.50.51.02.068.8～95.39.3～19.50.950～0.997NitroimidazoleMetronidazole0.51.02.04.071.1～90.35.8～18.80.932～0.992Dimetridazole0.51.02.04.070.4～92.43.2～16.30.943～0.999Ronidazole0.51.02.04.064.9～89.69.8～15.30.917～0.982765r0.9072。A%=SlopesSlopemax×100SlopesSlopemax5。。21RSD50%2。、、。。3.3.32.3.12.3.2。、、、1.02.04.0μg/kg5.010.020.0μg/kg0.51.02.0μg/kgβ-20.0μg/kg40.0μg/kg80.0μg/kg。2http//。7659.4%～111.6%2.6%～27.3%n=6。5。3.4231976110.926.5μg/kg。3。22338。221、、、、Fig.2Relativeslopeofsamplematrixfor21representativecompundsinshrimpmeatlivereggandmilk1.Sulfaguanidine2.Sulfaquinoxaline3.Sulfabenzamide4.Sulfacet-amide5.Bromazepam6.Diazepam7.Nitraz