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  • Ion Exclusion Chromatography a potentially valuable tool for fractionation

    of complex fluids: Juice de-acidification as a case study

    Dr Nikos Mavroudis

    Dept. of Applied Sciences, Faculty of Health & Life Sciences

    Northumbria University, Newcastle-upon-tyne, United Kingdom

    [email protected]

    +44-191-2437984

    mailto:[email protected]

  • Northumbria University is the largest university in the North East of England. 210m Annual budget 35,000 students from 140 countries make Northumbria the UKs sixth largest HE provider 17m is being invested in new research-active staff over three years.

    http://www.google.co.uk/url?sa=i&rct=j&q=uk+map+with+newcastle&source=images&cd=&cad=rja&docid=LfuW3YHxIqMZdM&tbnid=P2DQN8DMZudIfM:&ved=0CAUQjRw&url=http://conferences.ncl.ac.uk/igsm2011/location.php&ei=YA9jUdr6MOSV0AW-woCAAg&bvm=bv.44770516,d.d2k&psig=AFQjCNHIoECd2PQ2dZjyhGEh5SLqTIydPg&ust=1365532859475772

  • Introduction: More for Less

    Circular/Biobased Economy

    Biorefinery enabler

    Complex fluid fractionation process toolbox

    Cost effective (Food) functional ingredients

    Improving (Food) product quality

  • Introduction: Improving juice quality

    Fruit Juice quality and de-acidification acid/sugar ratio defines quality, and juices with high acid content

    are of reduced commercial value.

    Oxalic acid is considered an anti-nutrient and its removal would be a positive nutritional improvement.

    to maintain Juice status demands only minimal processing

    Tool: Ion Exclusion Chromatography, IEC applications from laboratory to industrial scale separations.

    Coupling IEC with advanced design chemical engineering approaches for industrial chromatography (Mazzotti-Morbidelli triangle theory) has the potential to be a valuable tool for generating natural fractions

  • IEC - animation Neutral molecule Charged molecule

    Co

    nce

    ntratio

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    Elution Time or [ Volume or Bed Volume]

    Detection

  • Objective

    Evaluate the ability of partial or total de-acidification in fruit juices using batch IEC.

    Infer about the de-acidification ability when Simulating Moving Bed (SMB) chromatography is used by calculating the complete separation region using the Mazzoti-Morbidelli triangle theory.

  • Materials and Methods

    Hardware Conditions

    Knauer simulating moving bed chromatography rig,was

    used in batch mode for the IEC experiments

    UBK530 ion exchange resin was packed in 75cm long

    column of 2cm ID.

    Packed column volume [Bed Volume] = 235.6 mL

    Injection of juice was 12mL i.e. 5% of the BV

    Experiments were run at 2.5 and 5mL/min volumetric

    flow rate and ambient temperature.

    Demineralised water has been used as eluent.

    Knauer HPLC with RI and UV detectors

    Fractions collected were analysed for sugars and acids

    using an Aminex column, 0.005N H3PO4 eluent at 35oC

    and at 0.3mL/min. Chromatograms were analysed using

    the Elite Chromgate software.

    To infer the ability for successful separation of targeted acids from sugars in high yields and purity using SMB, Henry coefficients were calculated from HPLC analysis (Francotte et al., 1998 Journal of Chromatography A 796, 239-248.).

  • 0.0

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    Sucrose g/L _ 2.5mL/min

    Glucose g/L _ 2.5mL/min

    Fructose g/L _ 2.5mL/min

    Oxalate g/L _ 2.5mL/min

    Citrate g/L _ 2.5mL/min

    Malate g/L _ 2.5mL/min

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    Glucose g/L _ 5 ml/min

    Fructose g/L _5mL/min

    Sucrose g/L_ 5mL/min

    Oxalate g/L _ 5mL/min

    Citrate g/L _ 5mL/min

    Malate g/L _ 5mL/min

    2.5 mL/min elution speed

    5 mL/min elution speed

    APPLE JUICE FRACTIONATION RESULTS, Orange and Beetroot juices were similar.

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    Malate AJE 44_20_2.5

    Citrate AJE 44_20_2.5

    Oxalate AJE 44_20_2.5

    Sucrose AJE 44_20_2.5

    Glucose AJE 44_20_2.5

    Fructose AJE 44_20_2.5

    Apple juice IEC @20C &2.5mL/min Effect of feed concentration

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    Malate AJE 22_20_2.5 (g/L)

    Citrate AJE 22_20_2.5 (g/L)

    Oxalate AJE_22_20_2.5 (g/L)

    Sucrose AJE 22_20_2.5 (g/L)

    Glucose AJE 22_20_2.5 (g/L)

    Fructose AJE 22_20_2.5 (g/L)

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    Malate AJE_11_20_2.5 (g/L)

    Citrate AJE_11_20_2.5 (g/L)

    Oxalate AJE_11_20_2.5 (g/L)

    Sucrose AJE_11_20_2.5 (g/L)

    Glucose AJE_11_20_2.5 (g/L)

    Fructose AJE_11_20_2.5 (g/L)

    11% solids

    22 % solids

    44 % solids

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    Elution time in Bed Volume

    Sucrose g/L _ 2.5mL/min

    Glucose g/L _ 2.5mL/min

    Fructose g/L _ 2.5mL/min

    Oxalate g/L _ 2.5mL/min

    Citrate g/L _ 2.5mL/min

    Malate g/L _ 2.5mL/min

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    Con

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    in g

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    Elution time in Bed Volume

    Glucose g/L _ 5 ml/min

    Fructose g/L _5mL/min

    Sucrose g/L_ 5mL/min

    Oxalate g/L _ 5mL/min

    Citrate g/L _ 5mL/min

    Malate g/L _ 5mL/min

    2.5 mL/min Elution speed

    5 mL/min elution speed

    Batch Chromatography Results Corresponding complete separation region after Mazzotti-Morbidelli SMB triangle theory

  • Conclusions

    IEC can be a helpful tool for partial or total deacidification of juices, without inducing chemical contaminants

    Based on the triangle theory, complete deacidification is possible when using SMB [a continuous chromatographic process based on the IEC mechanisms].

  • further work

    Effect of temperature

    Validation trial with Knauer SMB rig.

  • THANK YOU !

    Acknowledgements Financial support from Knauer GmbH and Northumbria Uni. R&D Funds.

    Prof. Marco Mazzotti, ETH-Zurich, for introducing me into Simulating Moving

    Bed Chromatography design theory for multi-component complex fluids