高效液相色谱法测定卷烟主流烟气中巴豆醛

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©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(),2009,31(S1):305309CN53-1045/NISSN0258-7971JournalofYunnanUniversityX1,2,2,2,1(11,650091;21,650106):.(2,4-),2%-,NovapaKC18(waters,3mm150mm,415m),365nm.10gL-1,97176%,(RSD)2193%,016410122gmL-1,(R2)019999..7,.:;;2,4-;:O65717:A:0258-7971(2009)S1-0305-05,,,[1].D1HoffmanS1S1Hecht,[2].,7[3].,.[48],,,[68],.(2,4--),2%..7,.(7).1111(Waters996PDA,)(Wa2tersAlliance269,);(CERULEANSM410,);(ElmaTRANSSON2ICT890/H,);(WTCbinder,);(Whatman,);AB204-S(METTLERTOLEDO,011mg);13mm0145m();(TH72-HTPWQ1,).()-DNPH(99%,ChemService);(,Merck);(,18k).2%().(60%62%)();2,4-(DNPH)(,);();.(1182molL-1):100mLX:2009-01-08:(2001PY001).:(1978-),,,,.:,,,,.©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(A)50mL,20mL(60%62%),.-(01046molL-1):1182molL-1215mL100mL(A),11(V/V)/.DNPH(75mmolL-1):715gDNPH,300mL500mL(A),2215mL1182molL-1,DNPH,.112:,2mLDNPH(75mmolL-1),.:(221)(60%2%)48h,GB/T196092004.1131mL01046molL-1--,.22(1)60%(2%)[5],,2.35mL,2s,60s1,,2.,50mL,25mL2%()25mL,15min,30min0145m2mL.,.,,113,,.114:WatersNovapakC18(319mm150mm);:110mLmin-1;:30;:10L;A,B015%;:010min,42%A49%;1018min,49%A;1819min,49%A100%;1925min,100%A42%A.:365nm.1(b).1(a)-DNPH(b)Fig11Chromatogramsofcrotonaldehyde2,4-dinitrophenylhydrazonestandard(a)andcigarettesample(b)221121111DNPH1,DNPH.,DNPH,,DNPH50100mmolL-1,.DNPH75mmolL-1,75mmolL-1DNPH.211121,,2%()([7]).,,,25mL,30174g603()31©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(1mL[7],,).DNPH01182molL-101046molL-1-(VV=11),1mL01046molL-1-(VV=11),,01046molL-1-(VV=11)1mL,.1Tab11Theeffectofdifferentconcentrationsofderivati2zationreagentanddifferentamountofextractionsolventc(DNPH)/(mmolL-1)()/(g-1)V()/mL()/(g-1)2517126102618750291812027131753111425301741002710150291692Tab12TheStandardcurveandreproducibilityofCrotonaldehydeR2/(gmL-1)/(gmL-1)(S/N=3)/(g-1)RSD/%y=1198105x+41121020199990164101221029125,28103,29164,28134,301302193Y,X.21114,[68](///).,015%.212113,5,12,24,48h,.5RSD0158%,,2d.213-DNPH,2%(),(-DNPH)0164,1128,2156,5111,10122gmL-1,,.2,,,(R2)019999,,1(a).,5L,3,(-DNPH)10gL-1.214113,5,2.,5(RSD)2193%,.,1mL-DNPH,113,,,3.597176%,.215113[7],4.,703S1:©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.[7].3Tab13Therecoveryofcrotonaldehyde/(g-1)/g/(g-1)/%12911210671499215229112207911910417532911230871669810742911240951949412552911250107186991244(:g-1)Tab14Contentsofdifferentmethods(unit:gpercigarrette)[7]12315515105224178161843231441613242515314199525102121015Tab15Resultsofcrotonaldehydeinmainstreamsmokeofdifferentbrands(unit:gpercigarrette)/(g-1)/(g-1)1#17211802#15231663#15261174#15241215#14201156#17251797#8111872161137,5.,,,,(7#).3(7),,[7],7.,,,[7]..:[1].[M].:,1992.[2]HoffmannD.Tobaccosmokecomponents.BeiZurTabInt,1998,23(1):49252.[3].[C]//,2003,1233.[4]Miyake,Takashi,Yashuhara,etal,GasChromatographicanalysisofacroleinas1-methyl-2-pyrazolineincigarettesmoke[J].KankyoKagaku,1995,5(3):569273.[5]DONGJi2zhou,SerbancMoldoveanu.Gaschromato2graphy-massspectrometryofcarbonylcompoundsincigaretemainstreamsmokeafterderivationwith2,4-dinitrophenylhydrazine[J].Journalofchromatography,2004,1027:25235.[6],,,.[J].,2006,12(5):15224.[7],,,.[J].,2007,25(2):2302233.[8],,,.[J].,2006,25(6):6782682.803()31©1994-2010ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.(11SchoolofChemistryScienceandEngineering,YunnanUniversity,Kunming650091,China;21YunnanReascendTobaccoTechnology(Group)Co1Ltd,Kunming650106,China)Abstract:Thedeterminationofcrotonaldehydeinmainstreamsmokebyhighperformanceliquidchro2matographywasinvestigated.ThecigarettesmokewascollectedusingaCambridgefiltertreatedwithacidicsolutionof2,4-dinitrophenylhydrazine.Crotonaldehyde-DNPHwasextractedfromtheCambridgefilterwith25mLof2%pyridineacetonitrilesolution.Crotonaldehyde-DNPHinsampleswasseparatedonNova2paKC18column(waters319mm15mm,415m)anddeterminedbydiodearraydetectorat365nm.Thedetectionlimitwas10gL-1,therecoverywas97176%,therelativestandarddeviation(RSD)was2193%,thelinearrangewas016410122gmL-1andthecorrelationcoefficient(R2)was019999.Themethodissimple,sensitiveandaccurate.Sevenbrandsofcigaretteweredeterminedandtheresultswerecontent.Keywords:crotonaldehyde;mainstreamsmoke;2,4-dinitrophenylhydrazine;highperformanceliquidchromatography333333333333333333333333333333333(304)CorrosioninhibitionofNeosinocalamumsaffinisleavesextractiveforsteelinHClsolutionLIXiang2hong,FUHui,XIAOXu2ping(DepartmentofFundamentalCourses,SouthwestForestryUniversity,Kunming650224,China)Abstract:SolidextractivefromNeosinocalamusaffinisleaveswasinvestigatedasanexcellentenviron2mentally-friendlyplantinhibitor.Theinhibitioneffectoftheplantextractiveonthecorrosionofcoldrolledsteel(CRS)in110mol/LHClhasbeenstudiedbyweightlossandTafelpolarizationmeth

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