顶空固相微萃取气相色谱法测定废水中挥发性脂肪酸冯琳

PTCA(PARTB:CHEM.ANAL.)2011471-(,400047):提出了顶空固相微萃取-气相色谱法测定废水中挥发性脂肪酸(乙酸丙酸丁酸戊酸异戊酸和己酸)的含量为使固相微萃取达到更高的效率,选择极性85mPA作为微萃取头的涂层,微萃取系在pH1.5的试液中进行,萃取温度及时间为25和20min,在20mL试样溶液中加入氯化钠3.5g作为盐析剂用Stabilwax-DA毛细管色谱柱分离,火焰离子检测器检测6种脂肪酸在一定的质量浓度范围内与其峰面积呈线性关系,相对标准偏差(n=10)均小于10.0%:气相色谱法;顶空固相微萃取;挥发性脂肪酸;废水:O657.7:A:1001-4020(2011)01-0086-04GCDeterminationofVolatileFattyAcidsinWasteWaterwithHS-SPMEFENGLin(CollegeofChem.,ChongqingNormalUniversity,Chongqing400047,China)Abstract:GCwithheadspace-solidphasemicro-extraction(HS-SPME)wasappliedtothedeterminationof6fattyacids,i.e.,aceticacid,propionicacid,butyricacid,pentanoicacid,isopentanoicacidandhextanoicacid,inwastewater.ToattainahigherefficiencyinSPME,thepolar85mPAcoatingwasselectedforthemicro-extractor,andtheextractionwascarriedoutat25for20minfromthesamplesolutionhavingtheacidityofpH1.5,andwithadditionof3.5gofNaClto20mLofsamplesolutionassaltingoutagent.TheanalytewereseparatedwithStabilwax-DAcapillarycolumnanddetectedbyFID.Linearrelationshipsbetweenvaluesofpeakareaandmassconcentrationof6fattyacidswerekeptindefiniteranges.ValuesofRSDs(n=10)ofthe6fattyacidsfoundwerelessthan10.0%.Keywords:GC;HS-SPME;Volatilefattyacids;Wastewater(VFAs),[1]()[2-3],,,,[4]:2009-11-19:(09XLB023):(1963-),,,,,,(GC)(FID),,,,[5](HS-SPME),,,[6]SPME[7],-(CW-DVB)SPME,-(GC-MS)[8],-(PDMS-86:-CAR)SPME,GC-FID[9]GC[10],HS-SPME,,,11.1TRACEGC;85-2;S-3DpH;40mL:2-1250~2500mgL-1,2-250mgL-1;60mgL-1,4,:1427.6gL-12-,1.2Stabilwax-DA(30m0.32mm,0.5m)(99.999%),1.2mLmin-1;(99.999%),280,250,,1min;,1.2mLmin-1;70,2min,4min-1180,2min,20min-1200,3min1.32h,30min20mL(pH1.5)40mL,2-(,pH1.5),SPMESPME250,3min322.11(a)(b)1.2.3.4.5.6.2-7.1(a)(b)Fig.1Chromatogramsofstandardsolution(a)andwastewatersample(b)2.22.2.1萃取涂层,,85m(PA)65mCW-DVB65m-(PDMS-DVB)75mPDMS-CAR4:CW-DVB,,PA,CW-DVB[11],85mPA87:-2.2.2萃取温度:25,;25,2-,20~45[11]2-,,PA,252.2.3萃取时间:,2-,,,20min2.2.4酸度pH:pHPA,,pH1.0,[7]pH1.52.2.5盐效应,:,;3.5~5.5g,2-,3.5g,2-,3.5g,20mL3.5g2.3,110,4.9%~9.8%467,62,19,12,3,3gL-11Tab.1Linearityranges,linearregressionequationsandcorrelationcoefficientsofthevolatilefattyacids/(gL-1)y=0.0404+1.474x1500~400000.9913y=-0.0154+1.35810-4x70~450000.9954y=-0.0998+5.87310-4x10~350000.9968y=-0.049+8.65810-4x55~60000.9986y=-0.139+4.19710-4x15~60000.9987y=-0.156+5.94110-3x15~55000.99982.420mL,,:2842,1733.9,2115.5,376.1,430.0,436.4gL-1,99.9%,96.1%,104.2%,97.3%,101.7%,89.1%2.5,22:,,,,2Tab.2AnalyticalresultsofsamplesmgL-1342514124.82.52.71.80.80.10.30.117125.12.01.30.71.20.70.10.050.120.0588:-:[1]CAIM,LIUJ,WEIY.Enhancedbiohydrogenpro-ductionfromsewagesludgewithalkalinepretreatment[J].EnvironSciTechnol,2004,38(11):3195-3202.[2]CHENY,RANDALLAA,MCCUET.Theeff-iciencyofenhancedbiologicalphosphorusremovalfromrealwastewateraffectedbydifferentratiosofacetictopropionicacid[J].WaterRes,2004,38(1):27-36.[3]TAKAIT,HIRATAA,YAMAUCHIK,etal.Effectsoftemperatureandvolatilefattyacidsonnitr-ification-denitrificationactivityinsmal-lscaleanaerobic-aerobicrecirculationbiofilmprocess[J].WaterSciTechnol,1997,35(6):101-108.[4]VENKATAMS,CANDRASEKHARARN,KRISHNAPK,etal.Anaerobictreatmentofcom-plexchemicalwastewaterinasequencingbatchbiofilmreactor:processoptimizationandevaluationoffactorinteractionsusingthetaguchidynamicDOEmethodo-logy[J].BiotechnologyandBioengineering,2005,90(6):732-745.[5]PANL,PAWLISZYNJ.Derivatization/solid-phasemicroextraction:newapproachtopolaranalytes[J].AnalChem,1997,69(2):196-205.[6],,,.[6][J].,2007,35(9):1269-1273.[7]PANL,ADAMSM,PAWLISZYNJ.Determinationoffattyacidsusingsolid-phasemicroextraction[J].A-nalChem,1995,67(23):4396-4400.[8]YOSP.Analysisofvolatilefattyacidsinwastewatercollectedfromapigfarmbyasolidphasemicroextrac-tionmethod[J].Chemosphere,1999,38(4):823-834.[9]ABALOSM,BAYONAJM,PAWLISZYNJ.Deve-lopmentofaheadspacesolid-phasemicroextractionprocedureforthedeterminationoffreevolatilefattyacidsinwastewaters[J].JChromatogrA,2000,873(1):107-115.[10]ABALOSM,BAYONAJM.Applicationofgaschromatographycoupledtochemicalionizationmassspectrometryfollowingheadspacesolid-phasemicro-extractionforthedeterminationoffreevolatilefattyacidsinaqueoussamples[J].JChromatogrA,2000,891(2):287-294.[11]MILLSGA,WALKERV,MUGHALH.Head-spacesolid-phasemicroextractionwith1-pyrenyld-iazomethanein-fibrederivatisationforanalysisoffae-calshort-chainfattyacids[J].JChromatogrB,1999,730(1):113-122.[12]PINHOO,FERREIRAI,FERREIRAMA.Solid-phasemicroextractionincombinationwithGC-MSforquantificationofthemajorvolatilefreefattyacidsinewecheese[J].AnalChem,2002,74(20):5199-520.(上接第85页):[1],,.[J].,2006,55(6):623-625.[2].[M].:,1972:187-189.[3],,,.[J].,2007,29(5):50-51.[4].(Mg40SiFe)[J].,2000,152(3):37-39.[5],,.[J].,2004,25(3):16-19.[6],.[J].,1999,110(2):13-14,43.[7].[M].:,1979:205.2011,:-20115,E-mail:[e-mail],;:,:214151,:,:0510-83712242,1390619703989