INQUISAL   20936
INSTITUTO DE QUIMICA DE SAN LUIS "DR. ROBERTO ANTONIO OLSINA"
Unidad Ejecutora - UE
artículos
Título:
Optimization ofultrasoundassisted-emulsification-dispersiveliquidliquid
Autor/es:
VIVIANA P.JOFRÉ A.; MARIELAV.ASSOF.; MARTÍNL.FANZONEA,; HÉCTORC.GOICOECHEAB. MARÍA F.SILVA B,C; LUIS D. MARTINEZ
Revista:
ANALYTICA CHIMICA ACTA
Editorial:
ELSEVIER SCIENCE BV
Referencias:
Año: 2010 p. 100 - 105
ISSN:
0003-2670
Resumen:
A newmethodwasdevelopedforanalyzingsulfurcompoundsinthearomaofwhitewines using ultrasoundassisted-emulsification-dispersiveliquidliquidmicroextractioncoupledwithgas chromatographymass spectrometrydetection.Inthepresentwork,theanalyticalmethodforsimultane- ous determinationofsevensulfurcompounds(methylmercaptoacetate,methyl(methylthio)acetate,2- methylthioethanol, 3-methylthiopropanol,3-methylthiohexanol,4-methylthio-4-methyl-2-pentanone and hexanethiol)isreported.Parametersthataffecttheefficiencyofthemethodologysuchasextract- ing anddispersingsolvents,samplevolume,ionstrength,cavitationtimeandcentrifugationtimewere investigated usingafractionatedfactorial261 (R =V)screeningdesign.Then,thefactorspresentingsig- nificant positiveeffectsontheanalyticalresponse(extractingvolume,ionstrength,cavitationtimeand centrifugation time)wereconsideredinafurthercentralcompositedesigntooptimizetheoperational conditions fortheultrasoundassisted-emulsification-dispersiveliquidliquidmicroextractionproce- dure. Additionally,multipleresponsesimultaneousoptimizationbyusingthedesirabilityfunctionwas used tofindtheoptimumexperimentalconditions.ThebestresultswereobtainedusingpHsample 4.25, extractantvolume150 L, ionicstrength8.75%NaCl,cavitationtime20sandcentrifugationtime 50 s.Theuseoftheoptimizedultrasoundassisted-emulsification-dispersiveliquidliquidmicroextrac- tion techniqueallowedtoobtainthebestextractionresultswiththeminimuminterferencefromother substances fromthematrix,anditallowedtoquantifytheanalytesinwhitewinesamplesbycalibration graphs. Recoveriesrangingfrom91.99%to125.87%forallsulfurcompoundsprovedtheaccuracyofthe proposed methodinwhitewinesamples.Methoddetectionlimitswereintherangeof0.361.67ngmL−1 and limitsofquantitationwerebetween0.63and3.02ngmL−1 for sulfurcompoundsinwhitewinesam- ples. Theproposedmethodologywassuccessfullyappliedforthedeterminationconcentrationsofsulfur compounds indifferentcommercialChardonnaywinesamplesfromMendoza,Argentine. © 2010 Elsevier B.V. All rights reserved 61 (R =V)screeningdesign.Then,thefactorspresentingsig- nificant positiveeffectsontheanalyticalresponse(extractingvolume,ionstrength,cavitationtimeand centrifugation time)wereconsideredinafurthercentralcompositedesigntooptimizetheoperational conditions fortheultrasoundassisted-emulsification-dispersiveliquidliquidmicroextractionproce- dure. Additionally,multipleresponsesimultaneousoptimizationbyusingthedesirabilityfunctionwas used tofindtheoptimumexperimentalconditions.ThebestresultswereobtainedusingpHsample 4.25, extractantvolume150 L, ionicstrength8.75%NaCl,cavitationtime20sandcentrifugationtime 50 s.Theuseoftheoptimizedultrasoundassisted-emulsification-dispersiveliquidliquidmicroextrac- tion techniqueallowedtoobtainthebestextractionresultswiththeminimuminterferencefromother substances fromthematrix,anditallowedtoquantifytheanalytesinwhitewinesamplesbycalibration graphs. Recoveriesrangingfrom91.99%to125.87%forallsulfurcompoundsprovedtheaccuracyofthe proposed methodinwhitewinesamples.Methoddetectionlimitswereintherangeof0.361.67ngmL−1 and limitsofquantitationwerebetween0.63and3.02ngmL−1 for sulfurcompoundsinwhitewinesam- ples. Theproposedmethodologywassuccessfullyappliedforthedeterminationconcentrationsofsulfur compounds indifferentcommercialChardonnaywinesamplesfromMendoza,Argentine. © 2010 Elsevier B.V. All rights reserved