沉积物中有机氯农药超声提取分析方法研究

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,3,,,100012:(OCPs),GC-ECD.11OCPs(,-HCH,-HCH,,,-HCH,-HCH,p,p-DDE,o,p-DDT,p,p-DDDp,p-DDT),OCPs:P(11),60min,1,DB-1701,GC-ECD,70%,(USEPA).OCPs.,,-HCH,-HCH,,-HCH,-HCH,p,p-DDE,o,p-DDT,p,p-DDDp,p-DDT;DDTsp,p-DDT,DDE;HCHs-HCH.,HCHs,DDTs.:;;:X522:A:1001-6929(2008)03-0135-06StudyontheUltrasonicExtractionMethodofOrganochlorinePesticidesintheSedimentsLURui,QINYan2wen,ZHENGBing2hui,ZHANGLeiRiverandCoastalEnvironmentalResearchCenter,ChineseResearchAcademyofEnvironmentalSciences,Beijing100012,ChinaAbstract:TheOCPsofthesedimentsweredistilledwiththeultrasonicextractionmethodandmeasuredbyGC2ECD.Theextractionconditionswereoptimizedbycomparisonwithseveralorganicsolvents,thedurationofultrasonic,thestepsofextractionandthedifferentGCcolumns.Resultsshowedthattheoptimalconditionswereobtainedusingthemixtureofhexaneanddichlormethane(11)inonestepfor60minsandtherecoveriesofOCPswereallabove70%,whichcouldmeettherequestofUSEPA.Hexachlorobenzene,2HCH,2HCH,heptachlor,2HCH,2HCH,p,p2DDE,o,p2DDT,p,p2DDD,p,p2DDTinthesamplescollectedfromLiaodongBaywerealldetectedusingtheaboveoptimalconditions.Thep,p2DDTand2HCHwerethedominatingcomponentsoftheDDTsandHCHsinthesedimentstakenfromLiaodongBay,respectively.ComparedwithotherriverPestuarysediments,theconcentrationsofHCHs,DDTsandhexachlorobenzeneinsedimentsfromLiaodongBaywerehigher,whichillustratedthatthecontaminationofOCPswasseriousinLiaodongBay.Keywords:organochlorinepesticides;sediment;ultrasonicextraction:2007-08-23:2007-10-11:(973)(2007CB407306);(40406026):(1982-),,,,ruilu2018@163.com.3,wittyqin@126.com(OrganochlorinePesticides,OCPs),:,;,.1983,,,,.(USEPA)13,68[1],2001,12[2].,[324],.OCPsUSEPAEPA8081A.,.213ResearchofEnvironmentalSciencesVol.21,No.3,2008,,[5];,,,[629].OCPs(),OCPs,OCPs.11.120069,1..,100(01149mm),.1Table1Thelongitudeandlatitudeofthesamplingsites1()1222950.041046.621222016.1405842.431220653.0404652.21.2GC2010-ECD63Ni.:HP-5(30m0132mm0125m);DB-1701(30m0132mm0125m).J.T.Baker,;FisherScientific,;Tedia,.:-HCH,-HCH,-HCH,-HCH,p,p-DDD,p,p-DDE,p,p-DDTo,p-DDT8;.(PCB209),SupelcoCo.(CatNo.48460).1.3,3120mLPmin,,1L,.220,280.:802min,10Pmin160,4Pmin230,10Pmin280,10min..1.4,,OCPs,.1.4.1OCPsHP-5(30m0132mm0125m)DB-1701(30m0132mm0125m).1.4.2(P(11)P(41)P(11)),2g,20mL,120min,,30min,15min(1000rPmin),15min,K-D,,1mLGC.1.4.32gOCPs,20mLP(11),30,60,90120min,1,3,11412.1.4.42gOCPs,20mLP(11),60min,13,3,11412.1.5(-HCH,-HCH,-HCH,-HCH,p,p-DDD,p,p-DDE,p,p-DDT,o,p-DDT,,,),,114.1.62g,114(11412)OCPs.22.1OCPs,,(2,4,10,20,40,60gPL),2,,r20199.63121OCPs12.1-HCH;2;3-HCH;4-HCH;5-HCH;6;7;8p,p-DDE;9p,p-DDD;10o,p-DDT;11p,p-DDT1HP-5OCPsGC-ECDFig.1Chromatogramoforganochlorinepesticidesstandards(GCcolumn:HP25)1;2-HCH;3-HCH;4;5;6-HCH;7-HCH;8p,p-DDE;9o,p-DDT;10p,p-DDD;11p,p-DDT2DB-1701OCPsGC-ECDFig.2Chromatogramoforganochlorinepesticidesstandards(GCcolumn:DB21701)(R)[10]:R=2(tR2-tR1)P(W1+W2)(1),tR1tR212,min;W1W212.,R115,12.(1)1HP-5p,p-DDDo,p-DDT(R)016,p,p-DDDo,p-DDT.2DB-1701p,p-DDDo,p-DDT(R)319,,OCPs,.DB-1701.DB-1701,P(11),GC,,10,2.IUPAC(X=X+kSb,X;Sb;k,1975IUPACk3),GCDL(DL=kSbPk,k,).OCPsGC2.2OCPsTable2ThestandardcurveequationofOCPsanddetectionlimitr2P(gL-1)y=26882x+701360.99720.34-HCHy=25458x-115810.99970.74-HCHy=23896x-1521.10.99981.02y=43165x+6761.60.99990.73y=73751x+320140.99960.67-HCHy=12295x+499370.99661.04-HCHy=21390x-6421.80.99970.57p,p-DDEy=19495x+9083.20.99970.30o,p-DDTy=11447x-16500.99940.38p,p-DDDy=14952x+122520.99970.22p,p-DDTy=10104x-199850.99500.482.2OCPs,.OCPs,4.P(11)P(11)P(41),09418%,1713%11210%,51138%12310%,110%14519%(3).9717%,8515%,7312%13219%.,P(11),o,p-DDT(51138%),OCPs70%(3).2.3P(11),30,60,90120min,,60minOCPs(73%,o,p-DDT)(4).2.413,(3).,1,o,p-DDTOCPs7516%,1.7313:3Fig.3EffectofdifferentsolventsontheefficiencyoftheorganochlorinepesticidesextractionfromsedimentsPmin:130;260;390;41204Fig.4Effectofdifferenttimeontheefficiencyoftheorganochlorinepesticidesinthesediments2.5OCPs(,GC-ECD):DB-1701,P(11),60min,1.2.63:(),OCPs(4).4,,-HCH,-HCH,,-HCH,-HCH,p,p-DDE,o,p-DDT,p,p-DDDp,p-DDT.w(OCPs)281322714ngPg,13914ngPg.2.6.1,.3,,,83121.3Table3RecoveryofpesticidesfromthesedimentindifferentextractionstepsOCPsP%123USEPA[11]P%81.4123.9155.9-HCH103.2125.0170.437134-HCH113.0131.6144.219140103.6135.3162.63411180.044.249.342122-HCH86.3103.9128.717147-HCH120.6160.9183.732127p,p-DDE103.6127.8121.330145o,p-DDT32.928.322.9p,p-DDD112.9173.1162.331141p,p-DDT71.384.2161.2251604OCPsTable4ThelevelsofOCPsinthesedimentstakenfromLiaodongBayngPgOCPs-HCH18.911.11.810.61.818.9-HCH5.23.20.42.90.45.2-HCH38.267.017.741.017.767.0-HCH20.321.70.214.10.220.3HCHs82.682.620.168.620.1103.0p,p-DDE16.521.43.913.92.921.4o,p-DDT9.410.21.47.01.410.2p,p-DDD4.23.6nd2.6nd4.2p,p-DDT13.741.72.419.32.441.7DDTs43.876.97.742.87.776.936.041.1nd25.7nd41.1nd6.40.52.3nd6.4ndndndndndnd162.4227.428.3139.428.3227.4:;nd.2.6.2,w()2517ngPg,(w()1109ngPg[12],w()6181617ngPg(1119ngPg)[13],w()411ngPg[14]),.2.6.3HCHs3HCHs4,w(-HCH),4110ngPg,-HCH,w(-HCH)1411ngPg.HCHs,HCHs4:-HCH(60%70%),-HCH(5%12%),-HCH(10%15%)-HCH(6%10%)[15],HCHs:-HCH15145%,-HCH-HCH59177%20155%.-HCH,-HCH[16217].,HCHs,.2.6.4DDTs3,DDTso,p2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