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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

Ion Exclusion Chromatography a potentially valuable … · Ion Exclusion Chromatography a potentially valuable tool for fractionation of complex fluids: Juice de-acidification as

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Page 1: Ion Exclusion Chromatography a potentially valuable … · Ion Exclusion Chromatography a potentially valuable tool for fractionation of complex fluids: Juice de-acidification as

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

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

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Introduction: More for Less

• Circular/Biobased Economy

– Biorefinery enabler

• Complex fluid fractionation process toolbox

• Cost effective (Food) functional ingredients

• Improving (Food) product quality

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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

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IEC - animation Neutral molecule Charged molecule

Co

nce

ntratio

n

Elution Time or [ Volume or Bed Volume]

Detection

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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.

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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.).

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0.0

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0.0 0.2 0.4 0.6 0.8 1.0

Co

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g/L

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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2.0

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0.0 0.2 0.4 0.6 0.8 1.0 1.2

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g/L

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

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

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0.0 0.2 0.4 0.6 0.8 1.0 1.2

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on

in g

/L

Elution in Bed Volume

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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in g

/L

Elution in Bed Volume

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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/L

Elution in Bed Volume

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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0.0

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15.0

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25.0

0.0 0.2 0.4 0.6 0.8 1.0

Conc

entr

atio

n in

g/L

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

0.0

2.0

4.0

6.0

8.0

10.0

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16.0

18.0

0.0 0.2 0.4 0.6 0.8 1.0 1.2

Con

cen

trat

ion

in g

/L

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

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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].

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further work

• Effect of temperature

• Validation trial with Knauer SMB rig.

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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