固相萃取气相色谱法测定北京市水样中的邻苯二甲酸酯贾宁

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- ,,,, ,,, (,100022) :研究了使用毛细管柱(OV-1701)分离、FID作为检测器的气相色谱法测定水中5种邻苯二甲酸酯(PAEs)[邻苯二甲酸二乙酯(DEP),邻苯二甲酸二丁酯(DBP),邻苯二甲酸丁基苄基酯(BBP),邻苯二甲酸二(2-乙基己基)酯(DEHP),邻苯二甲酸二环己酯(DCHP)]的色谱条件。5种PAEs检出限在0.1~0.3μgL之间,所测PAEs的质量浓度在0.5~100μgL范围内,RSD在2.2%~3.3%之间,各物质校正曲线(质量浓度与峰面积)的相关系数在0.9970~0.9993之间。利用固相萃取技术萃取水中PAEs,回收率在82.5%~110.5%之间,RSD在1.1%~4.0%之间。北京市吴家村污水处理厂4个采样点中邻苯二甲酸酯浓度在(0.7~193.3)μgL之间。北京市南护城河的3个采样点中邻苯二甲酸酯浓度在(0.1~241.8)μgL之间。:邻苯二甲酸酯;环境激素;气相色谱法;固相萃取法:O657.7  :A   :1000-0720(2005)11-0018-04  (PAEs),[1],,,[2]。PAEs,、[3]。PAEs,、、、、、。PAEs,PAEs。,10-9[4],[5],PAEs,。PAEs。6PAEs129,(DMP)、(DEP)、(DBP)、(DOP)、(BBP)(2-)(DE-HP)。DMP、DBP、DOP。PAEs,(SPE)(SPME);(GC)(HPLC)。、,,、、、。[6]C18C18[7],PAEs。CaiYaqi[8](multi-walledcarbonnanotubespackedcartridge)DEP、DNPrP、DIBP、DCHP,,XDB-C8HPLC。0.18~0.86μgL,80.3%~104.5%。L.Brossa[9]-(polystyrene-divinylbenzene,PS-DVB)—18—2411200511            ChineseJournalofAnalysisLaboratory            Vol.24.No.112005-11:2004-11-02;:2005-04-13:(HBWDEP-2003-01): (1980-),,DOI:10.13595/j.cnki.issn1000-0720.2005.0253,SPE-GC-MS(--)PAEs。HideyukiKat-sumata[10]、PAEs(BBP、DBP、DCHP)。5PAEs(DEP、DBP、BBP、DEHPDCHP)。5PAEs、。。1 1.1 GC7890Ⅱ,FIDT2000();:SupelcoVisiprepTMDL;:WatersOASIS®HLB(6mL,200mg);:GASTMANUFACTUR-ING.INC.DOA-P104-BN。:150mm();:DHG-9003()。1.2 :(DEP,99.0%),(DBP,99.5%),(BBP,98.0%),(2-)(DEHP,99.4%),(DCHP,99.0%),ChemSer-vice(USA)。、();(400℃4h,);;;,99.99%()。1.3 DEP、DBP、BBP、DEHP、DCHP0.1000g,100mL,1000mgL。510mL100mL,,100mgL,4℃。100mgLPAEs,0.50、2.00、10.00、20.00、50.00、100.00mgL,4℃,0.50、2.00、10.00、20.00、50.00、100.00μgL。1.4 PAEs,。:1.HLB:(V()∶V()=95∶5)、、6mLHLB,HLB5min,,2~3mLmin。,,。2.:50KPa1LHLB,5mLmin,HLB,HLB。3.HLB:5mL(V()∶V()=95∶5)HLB。HLB3~5min,。4.:(V()∶V()=95∶5)9mL,HLB1min1mLmin,。,HLB。5.:1gNa2SO4,。6.:K-D,0.5mL,1mL,2mL,,。2 2.1 ,30m×0.32mm×0.33μmOV-1701;(99.99%);:280℃,(FID):280℃;:16mLmin;,:2.76∶1;,:16.28mLmin;():16mLmin;():150mLmin;4.0μL;:130℃,1min,10℃min260℃,8min。,。5PAEsDEP、DBP、BBP、DEHP、DCHP。—19—2411200511            ChineseJournalofAnalysisLaboratory            Vol.24.No.112005-111 5PAEsFig.1 GaschromatogramsoffivestandardPAEs2.2 0.50、2.00、10.00、20.00、50.00、100.00mgL“2.1”GC,yρ(mgL),,1。,5PAEsyρ(μgL),0.99。1 PAEs、Tab.1 RegrossionequationandcorrelationcoefficientforPAEsrDEPy=1266.0ρ-28450.9986DBPy=2611.6ρ-57460.9993BBPy=4412.0ρ-135880.9970DEHPy=5076.8ρ-172640.9971DCHPy=4450.8ρ-146890.99872.3 、(RSD)0.50、2.00、10.00、20.00、50.00、100.00μgL,“1.4”,“2.1”GC,,5PAEs、(2),20μgL,5,2。2.4 20.00μgL“1.4”,“2.1”GC,5,3。2.5 4:、、3:、、。5.0μm(,Υ150mm),1.0L,“1.4”,“2.1”GC45。2 、(RSD)Tab.2 DeterminationresultsforPAEsρ(μgL)RSD%(n=5)ρ(μgL)DEP0.13.00.5~100DBP0.13.10.5~100BBP0.12.20.5~100DEHP0.33.30.5~100DCHP0.32.40.5~1003 5PEAsTab.3 RecoveriesforfivePAEsρ(μgL)ρ(μgL)%RSD%(n=5)DEP20.0017.989.53.4DBP20.0022.1110.54.0BBP20.0018.592.31.1DEHP20.0016.582.53.6DCHP20.0018.190.72.54 PAEsρ(μgL)Tab.4 ContentsofPAEsamplesinWujiacunsewagetreat-mentplantDEP193.327.76.43.1DBP12.36.73.52.1BBPnd.nd.nd.nd.DEHP97.463.040.732.8DCHP2.91.70.7nd.∑PAEs305.999.151.338.0nd.:—20—2411200511            ChineseJournalofAnalysisLaboratory            Vol.24.No.112005-115 PAEsρ(μgL)Tab.5 ContentsofPAEsinwatersamplesofsouthmoatinBeijingDEP6.01.34.8DBP26.224.413.2BBPnd.nd.nd.DEHP241.8168.481.0DCHPnd.0.10.4∑PAEs274.0194.299.4nd.:4:4,DEP、DBP、DEHPDCHP,PAEs。DEPDEHPDBPDCHP;DEPDBPDEHP。4PAEs(0.7~193.3)μgL。GB8978-1996[11],GB3838Ⅲ,,DBP200μgL,DEHP300μgL,100%。5:PAEs。GB3838-2002[12],DBP3μgL,DEHP8μgL,0,100%。3,DBP(3~8)DEHP(9~29)DEP,DCHP;PAEs;PAEs;。,。PAEs。[1] MakotoEma,ReikoKurosaka,HiroAmanoetal.Toxicol-ogyLetters,1995,78(2):101[2] VanWA,VanV,PosthumusRetal.EcotoxicoEnvironSafety,2000,46:3205[3] ,,..1997,16(12):39[4] ,.().2004,15(2):52[5] ,,..2004,15(8):1455[6] ,,..2000,21(2):66[7] ,,..2000,20(2):146[8] CaiYaqi,JiangGuibin,LiuJingfu.AnalChimActa,2003,494:149[9] BrossaL,MarceRM,BorrullFetal.JournalofChroma-tographyA,2002,963:287[10] HideyukiKatsumata,AleyaBegum,SatoshiKanecoetal.AnalChimActa,2004,502:167[11] 、.GB8978-1996.1996[12] 、.GB3838-2002.2002DeterminationofthephthalatesinwatersamplesinBeijingcitybysolid-phaseextractionandgaschromatographyJIANing,XUHeng-zhi,HUYa-li,LINXing-tao,CHENMing,ZHANGShu-fen,WANGGui-huaandRENRen(CollegeofEnergyandEnviron-mentalEngineering,BeijingUniversityofTechnology,Beijing100022),FenxiShiyanshi,2005,24(11):18~21Abstract:Acapillarygaschromatographicmethodwithflameionizationdetector(GC-FID)forthedeterminationoffivephthalateacidesters(PAEs)(diethylphthalate(DEP),di-n-butylphthalate(DBP),butylbenzylphthalate(BBP),di(2-ethylhexyl)phthalate(DEHP),dicyclohexylphthalate(DCHP))inwatersampleswasdeveloped.Therewasagoodlinearrelationshipintherangeof0.5~100μgLwiththelowdetectionlimitsof0.1~0.3μgLandRSDof2.2%~3.3%.Therecov-eriesobtainedforPAEsrangedfrom82.5%to110.5%withRSDof1.1%~4.0%bysolid-phaseextraction.ThecontentsofPAEsinwatersamplesinWujiacunsew-agetreatmentplantvariedfrom0.7to193.3μgL.ThecontentsofPAEsinthewatersamplesofsouthmoatinBeijingvariedfrom0.1to241.8μgL.Keywords:Phthalateacidesters;Environmentalhor-mone;Capillarygaschromatography;Solid-phaseex-traction—21—2411200511            ChineseJournalofAnalysisLa

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