Fructo-oligosaccharides (FOS) namely, kestose, nystose and fructofuranosylnystose, are prebiotics that can be obtained by fermentation. The resulting fermentative broth is a complex mixture consisting also of salts and other sugars that must be removed. Adsorption equilibrium studies were conducted using the static method in batch mode onto Dowex Monosphere calcium resin, at 60ºC, for FOS contained in a fermentative broth and pure mixtures. Experimental isotherms data were analyzed using linear, Langmuir/anti-Langmuir, Freundlich, Redlich & Peterson, and Toth models. Isotherm parameters were determined using linear and nonlinear correlations for the minimization of several error functions. The nonlinear correlations were found to provide the best isotherm parameters for the models. FOS contained in a fermentative broth were well fitted with anti-Langmuir isotherms, while FOS in pure mixtures were better fitted with Toth, Langmuir and Redlich & Peterson isotherms. A detailed error analysis was carried out to investigate the effect of using different error criteria for the determination of the isotherm parameters

Nobre, Clarisse

Peres, A. M.

Polakovic, M.

Rodrigues, L. R.

Teixeira, J. A.

Vanková, K.

Vaňková, K.

Peres, António M.

Polakovič, M.

Teixeira, José

Rodrigues, Lígia R.

Biblioteca Digital do IPB

13th International Symposium onPreparative andIndustrialChromatography andAllied TechniquesScientific  ProgramSeptember 12    - 15   , 2010ththStockholm, Swedenwww.spica2010.seSPICA 2010 Stockholm 4110 Equilibrium studies for the adsorption of fructo-oligosaccharides from a pure mixture and a fermentative broth on a Dowex Monosphere calcium resin C. Nobre\* K.Vankova2, A. M. Peres3, M. Polakovic2, J. A. Teixeira\ L. R. Rodrigues1 1 IBB- Institute for Biotechnology and Bioengineering, Centre of Biological Engineering, University of Minho, Campus de Gualtar, 4710-057 Braga, Portugal 2 Department of Chemical and Biochemical Engineering, Institute of Chemical and Environmental Engineering, Faculty of Chemical and Food Technology, Slovak University of Technology, Radlinskeho 9, 812 37 Bratislava, Slovak Republic 3 LSRE - Laboratory of Separation and Reaction Engineering, Escola Superior Agraria - Institute Politecnico de Braganc;a, Quinta de Santa Apol6nia, Apartado 1172, 5301-855 Braganc;a, Portugal ABSTRACT Fructo-oligosaccharides (FOS) namely, kestose, nystose and fructofuranosylnystose, are prebiotics that can be obtained by fermentation. The resulting fermentative broth is a complex mixture consisting also of salts and other sugars that must be removed. Adsorption equilibrium studies were conducted using the static method in batch mode onto Dowex Monosphere calcium resin, at 60°C, for FOS contained in a fermentative broth and pure mixtures. Experimental isotherms data were analyzed using linear, Langmuirlanti-Langmuir, Freundlich , Redlich & Peterson, and Toth models. Isotherm parameters were determined using linear and nonlinear correlations for the minimization of several error functions. The non linear correlations were found to provide the best isotherm parameters for the models. FOS contained in a fermentative broth were well fitted with anti-Langmuir isotherms, while FOS in pure mixtures were better fitted with Toth, Langmuir and Redlich & Peterson isotherms. A detailed error analysis was carried out to investigate the effect of using different error criteria for the determination of the isotherm parameters. 157 -, ..... ... , -~ -~ , , ..._ ---~ ..... -------.._ .::: .: .: ... .: .. . .. 

Equilibrium studies of the adsorption of fructo-oligosaccharides from a pure mixture and a fermentative broth on a dowex monosphere calcium resin

Universidade do Minho: RepositoriUM

13th International Symposium onPreparative andIndustrialChromatography andAllied TechniquesScientific  ProgramSeptember 12    - 15   , 2010ththStockholm, Swedenwww.spica2010.seEquilibrium Studies of the Adsorption of Fructo-oligosaccharides from a Pure Mixture and a Fermentative Broth on aDowex Monosphere Calcium ResinC. Nobrea*, K.Vaňkováb, A. M. Peresc, M. Polakovičb, J. A. Teixeiraa, L. R. RodriguesaInstitute For Biotechnology And BioengineeringCENTRE OF BIOLOGICAL ENGINEERINGUNIVERSITY OF MINHOa IBB – Institute for Biotechnology and Bioengineering, Centre of Biological Engineering, University of Minho, Campus de Gualtar, Braga, Portugalb Department of Chemical and Biochemical Engineering, Institute of Chemical and Environmental Engineering, Faculty of Chemical and Food Technology, Slovak University of Technology, Bratislava, Slovak Republicc LSRE – Laboratory of Separation and Reaction Engineering, Escola Superior Agrária – Instituto Politécnico de Bragança, Bragança, PortugalE-mail*clarissenobre@deb.uminho.ptIntroduction Fructo-oligosaccharides (FOS) gained in the last years a large commercial interest due to its beneficial properties in the human health as prebiotics. Fermentative processes appear to be a good alternative for large scale production of FOS, that include kestose (GF2), nystose (GF3) and fructo-furanosylnystose (GF4).However, the result of such fermentations is a complex mixture containing salts and low molecular weight sugars such as glucose (G), fructose (F) and sucrose (GF), that do notcontribute to the beneficial effects and must be removed. Simulated moving bed chromatography (SMB) appears to be an efficient downstream process for the fractionation of sugars in an industrial scale. The major challenge whendesigning the separation process is the choice of an efficient ion-exchange resin. Therefore, the knowledge of the adsorption isotherms of the different compounds present inthe mixture is an important parameter to consider when selecting the resin. Moreover, the influence on the adsorption of salts and other sugars present in the mixture must bestudied. Modelling of the adsorption isotherms for FOS (from fermentative broth and pure mixtures) onto a Dowex Monosphere calcium resin. Determination of the model isotherm parameters using linear and non-linear correlations by minimization of several error functions.Static  - Adsorption /Desorption MethodResin CharacteristicsResin FOS solutions Adsorption Washing Desorption QuantificationHigh Performance Liquid Chromatography (HPLC)Dowex®Monosphere®99 Ca/320Tadsorption = 60 ºCContact time  = 8hCi: = 15 – 180 g/L    Vliquid  = 3.5 mL  Vadsorbent = 1.5 mLFermentative broth(38% FOS + 62% F, G, GF+ Calcium ions)Pure mixture(90% FOS + 10% F, G, GF)Decantation of the liquid phaseWashing the resin with pure waterAddition of 5mL of pure water Filtration of supernatant (0.2 µm)Horizontal shaking Horizontal shakingTadsorption = 25 ºCContact time  = overnightAimsExperimental MethodologyIsotherm ModelsDowex Monosphere 99Ca/320Ionic form Ca2+Structure Gel-typeMatrix Styrene-DVBFunctional group SulfonateTotal capacity (eq/L) >1.5 (H+ form)Water content (%) 57-61 (H+ form)Volume median  diameter (µm) 300-330Curvature Isotherm ModelLinear LinearUpward Anti-LangmuirDownwardLangmuirFreundlichRedlich & PetersonTothError FunctionSum square of the errors Hybrid fractional error functionMarquardt’s percent standard deviationAverage relative errorSum of absolute errorsLinear CorrelationIsotherm Parameters DeterminationNon-Linear CorrelationLinearization of the Model EquationsMinimization of several error functionsSmaller Sum of the ErrorsBest fitting of the experimantal dataResults0510152025300 20 40 60 80q [mg/g]C [g/L]Anti-LangmuirHenryExperimental0510152025300 20 40 60 80 100q [mg/g]C [g/L]Anti-LangmuirHenryExperimental01234560 5 10 15 20q [mg/g]C [g/L]Anti-LangmuirHenryExperimental05101520250 20 40 60 80q [mg/g]C [g/L]TothRedlich and PetersonFreundlichLangmuirHenryExperimentalPure Mixture051015200 20 40 60 80q [mg/g]C [g/L]TothRedlich and PetersonFreundlichHenryLangmuirExperimental0,00,51,01,52,02,50 2 4 6 8 10q [mg/g]C [g/L]TothRedlich and PetersonFreundlichLangmuirHenryConclusionsFermentative BrothGF2 GF3 GF4AcknowledgementsReferencesGF2 GF3 GF4Fermentative broth 0,36 0,29 0,26Pure mixture 0,35 0,28 0,25Linear Distribution coefficients (L.kg-1)C. Nobre acknowledges the F.C.T. - Fundação para a Ciência e a Tecnologia (Portugal) for the PhD Grant ref. SFRH/BD/32514/2006.   GR Gibson (2008) J Clin Gastroenterol 42:S75-S79 M Gramblicka, M Polakovic (2007) J Chem Eng Data 52:345-350 J Nowak, I Poplewska, D Antos, A Seidel-Morgenstern (2009) J Chrom A 1216:8697-8704 M Saska, MD Wu, SJ Clarke, K Iqbal (1992) Sep Sci Technol 27:1711-1732 M Hadi, MR Samarghandi, G Mckay (2010) Chem Eng J 160:408-416 FOS present in pure mixture or broth have different adsorption behaviors. High ionic strengths and high concentrations of the other sugars seems to influencethe adsorption. Toth, Langmuir and Redlich & Peterson isotherms were the models that bestrepresented the adsorption of FOS in the broth, while FOS in pure mixture were betterrepresented by the Anti-Langmuir isotherm. For both mixtures studied, the sugars were adsorbed according to their molecularsize and kept a constant selective behavior. The non-linear methods were found to be more adequate to estimated theisotherms parameters, being the HYBRID function the one that gives better the results.

Equilibrium studies of the adsorption of fructo-oligosaccharides from a pure mixture and a fermentative broth on a Dowex Monosphere calcium resin

Fructo-oligosaccharides (FOS) namely, kestose, nystose and
fructofuranosylnystose, are prebiotics that can be obtained by fermentation. The
resulting fermentative broth is a complex mixture consisting also of salts and
other sugars that must be removed. Adsorption equilibrium studies were
conducted using the static method in batch mode onto Dowex Monosphere
calcium resin, at 60ºC, for FOS contained in a fermentative broth and pure
mixtures. Experimental isotherms data were analyzed using linear,
Langmuir/anti-Langmuir, Freundlich, Redlich & Peterson, and Toth models.
Isotherm parameters were determined using linear and nonlinear correlations
for the minimization of several error functions. The nonlinear correlations were
found to provide the best isotherm parameters for the models. FOS contained in
a fermentative broth were well fitted with anti-Langmuir isotherms, while FOS in
pure mixtures were better fitted with Toth, Langmuir and Redlich & Peterson
isotherms. A detailed error analysis was carried out to investigate the effect of
using different error criteria for the determination of the isotherm parameters

Nobre, C.

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Equilibrium studies of the adsorption of fructo-oligosaccharides from a pure mixture and a fermentative broth on a Dowex Monosphere calcium resin

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