13 农药残留分析方法

1.1.2.2.3.3.4.4.5.5.2000200060060020002000,,60006000,,2600026000——11RRrodenticiderodenticidePGR/IPGR/IGRGRGrouwthGrouwthregulatorregulatorFuFufumigantfumigantHHherbicideherbicideFFfungicidefungicideAAacaricideacaricideNNnematicidenematicideIIInsecticideInsecticide——22FF[[--C(S)C(S)--SS--]As]AsasomateasomateFF--C(S)C(S)--SS--zinebzinebII(CH(CH33))22--NN--CHCH--(CH(CH22SSOSSO33H)H)22bisultapbisultapF/HF/H--NNcarbendazimcarbendazimIICHCH33--NHC(O)NHC(O)--ORORAldicarbAldicarbII--ClClFFBrBrCNCNdeltamethrindeltamethrinII(RO)(RO)33--POR=RPOR=R11/R/R22/R/R33]]trichlorfontrichlorfonI/AI/A--ClClDDTDDT//——22HHRR11--OCH2COCH2C--OROR22RR11==2,42,4--DD2,42,4--HH11--22CCNNparaquatparaquatHHRR11--NHNH--COCO--RR22alachloralachlorHH33CCNNatrazineatrazineHHRR11--NHC(O)NNHC(O)N--(R(R22))22chlorotoluronchlorotoluronFFCuSOCuSO44CopperCoppersulfatesulfate//1.2.3.4.5.1.1.----11ZZ----22SS2.2.(NY/T788(NY/T788--2004)2004)12L12kg05kg05kg12kg12kg12kg12kg12kg12kg3.3.250250500g500g11WWSSWWOO,,221.1.A.A.““””,,B.B.45458080,,C.C.,,,,D.D.,,,,E.E.——100100,,,,2.2.((EE——(1)(1)65,,,412,3,,2,,1——(2)(2)12345(SPE)7——(3)(3)GCHPLCGCHPLC1.-------2.-------SPME8——(4)(4)CO2NH3CH3OH.5GC....GCsupercricitalfluidextraction,SFE9——(5)(5)/GC/MS.—GC/MS..—GC/MS.10——(6)(6)C18,,,./HPLC../HPLC..HP50G..GC/MS2215.MSPDE11,,——1.1.——..////DMFDMF//DMSODMSO////2.2.FlorisilFlorisilAlAl22OO33FlorisilFlorisil,,FlorisilFlorisil..AlAl22OO33,,AlAl22OO33FlorisilFlorisil3.3.SolidPhaseExtraction,SPESolidPhaseExtraction,SPEPBAPBASAXSAXPSAPSANHNH22DEADEASCXSCXPRSPRSCBACBACNCN0H0HSiSiNHNH22PSAPSACC1818CC88CC22CHCHCNCNPHPH4.4.,,,,..5.5.//,,10ml10ml(20g(20g+360ml+360ml+40ml+40ml80%80%))10ml10ml/2ml/2ml(1g(1g+2ml+2ml180ml)180ml)10ml10ml(20g(20g+360ml+360ml+40ml80%+40ml80%))10ml10ml0.5mol/L0.5mol/L1.1.1717SERSSERS1616IRIR--ATRATR15151414CZECZE1313SFCSFC1212——1111——10109988776655443322112.2.----1010--10101010--1111ggFluorecenceFluorecenceDetectorDetectorFDFD1010--991010--1010ggUltravioletDetectorUltravioletDetectorUVUVPhotometryIonizationPhotometryIonizationDetectorDetectorPIDPIDAlkaliFlameIonizationAlkaliFlameIonizationDetectorDetectorAFIDAFID1010--10101010--1111ggNitrogenPhosphorousNitrogenPhosphorousDetectorDetectorNPDNPD1010--991010--1111ggFlamePhotometryDetectorFlamePhotometryDetectorFPDFPD1010--11111010--1212ggElectroCaptureDetectorElectroCaptureDetectorECDECDElectrolyticConductivityElectrolyticConductivityDetectorDetectorCoulometrieCoulometrieDetectorDetectorCDCD1010--1010ggFlameFlameThermionicThermionicDetectorDetectorFTDFTDFlameIonizationDetectorFlameIonizationDetectorFIDFIDThermalConductivityThermalConductivityDetectorDetectorTCDTCDC.M.TorresC.M.Torresetetal.J.Chromatographyal.J.ChromatographyA,1996(754):397A,1996(754):39717225243555158111111715113510217322168221179533117GC/MSMIP-AED/ELCDFPDNPDECD1.1.70%70%110%,110%,80%(n=5)80%(n=5),,353020151050-12060-12070-11070-11070-110%C0.0010.001C0.010.01C0.10.1C11(mg/kg)::MaximumResidueLevel,MaximumResidueLevel,MRLMRLLOQLOQ10LOQ10LOQCCLOQLOQ10LOQ10LOQMRLMRLLOQLOQMRLMRLCCLOQLOQMRLMRLMRLMRL2.2.(LOQ)(LOQ)limitofdetection,LODlimitofdetection,LODgg33ngngLOD=[3LOD=[3(H(HS)S)/(H/(HS)S)]]CCVV(H(HS)S)——(H(HS)S)——CC——((g/g/ll))VV——((ll))limitofquantification,LOQlimitofquantification,LOQmg/kgmg/kg,,LODLODmgmgllLOQ=LOQ=llkgkgLOQLOQLOQLOQ11MRL0.05mg/kgMRL0.05mg/kg,,LOQLOQ1/10MRL1/10MRL22MRLMRL0.05mg/kg0.05mg/kg,,LOQLOQMRLMRL1.01.00.50.50.20.20.10.10.10.10.040.040.020.020.020.020.010.010.0050.0050.0010.001LOQLOQ10105522110.50.50.20.20.10.10.050.050.020.020.010.010.0010.001MRLMRL3.3.MRLMRLFAO/WHOFAO/WHO,CCPR,CCPR199219920.50.5MRLMRL0.050.050.020.020.10.10.050.050.50.50.10.10.50.50.50.5550.50.555LPL/mg/kgLPL/mg/kgMRLMRL/mg/kg/mg/kg„„„„„„„„GC/MSGC/MSLC/MSLC/MS11707028d28d22g/kg22g/kg2.5g/kg2.5g/kg1.7g/kg1.7g/kg1.2g/kg1.2g/kg0.25g/kg0.25g/kg0.015g/kg0.015g/kg0.00020.0002WWOO13g/l13g/lWWSS310310224.9224.9CC66HH1010NN66CyromazineCyromazine::,,HPLCHPLC30g30ml,,Florisil1.5g/Envi-carb0.5g25ml31HPLC22WWOO12g/l12g/lWWSS220220HOHOP(O)P(O)--CH2CH2--NHNH--CH2CH2--COOHCOOHHOHOCC33HH88NONO55PPglyphosateglyphosate10g,5g0.5NH4HCO3H2O5gHPLC-SEP-PAK((POPsPOPs))1212PCDF-Clx(210)Polychlorinatedbiphenyl(PCDF)PCDDs-Clx(75)Polychlorinateddibenzofuran-PCBs-Clx(209)Polychlorinatedbiphenyl(PCBs)C10H7Cl7HeptachlorC6H6HexachlorobenzeneC12H12Cl12MirexC10H10Cl8CamphechlorC10H6Cl8ChlordaneC12H6Cl6AldrinC12H8Cl6OEndrinC12H8Cl6ODieldrinC14H9Cl5Dichlorodiphenyltrichloroethane----11GCGC--MS;MS;LCLC--MSMS--MSMSC18C18,,EnviEnvi--CarbCarb//SepSep--PakPak,,25ml25ml::(3:!)(3:!),,GCGC--ECDECD::4:14:1,,2%NaSO42%NaSO4GCGC--MS;MS;LCLC--MSMS--MSMSC18C18,,EnviEnvi--CarbCarb//SepSep--PakPak,,25ml25ml::(3:!)(3:!)::1:11:1;;,,CuCu::1:11:1333gFlorisil3gFlorisil,6%,6%--2211--1.5g1.5g10g10g+3ml+3ml,25ml,25mlXADXAD--22,,GCGC--ECDECD11----22GCGC--ECDECD,,1:11:1,,,,2%NaSO2%NaSO44,,,,..GCGC--ECDECD,,1111,,2%NaSO2%NaSO44GCGC--ECDECDCHCH22ClCl22NaSONaSO441111GCGC--MS;MS;LCLC--MSMS--MSMSBIOBIO--BeadsSBeadsS--X3X3NaSONaSO44,,::1111,,GCGC--ECDECD60%60%::1:11:19595--98982h,2h,11----31314588-Endosulfan-1