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Food Bioprocess Technol (2012) 5:2132-2139

DOI 10.1007M1947-011-0649-9

ORIGINAL PAPER

Discoloration Kinetics of Clarified Apple Juice Treated with Lewatit S


4528 Adsorbent Resin During Processing
Ibarz Albert Falguera Vctor Garza Salvador Garvn
Alfonso

Received: 6 September 2010/Accepted: 29 June 2011 /Published online: 13 July 2011


Springer Science+Business Media, LLC 2011

Abstract The present work studies the adsorption of colored


compounds in apple juice with a Lewatit resin S 4528. The
sorption equilibrium through the adsorption isotherms for 20, 35,
and 50 C was studied. The absorbance at 420 nm was used to
measure the concentration of colored compounds, which permits
correlating the residual concentration with the adsorbed
concentration, proving that the data matched reasonably well
according to the Langmuir and Freundlich models. Also, the
efficiency of the adsorption process was studied for different
resin/ juice mass ratios at different temperatures, from which it
was observed that there was an improvement in efficiency as the
resin content increased, while the increase in temperature was not
so important in the process. The adsorption kinetics at 35 C for
different resin/juice mass ratios was also studied. The kinetic
model developed by Ibarz was used, concluding that the data
matched this model reasonably well. The adsorption kinetic
constant was always higher than the desorption kinetic constant,
which indicates that the adsorption stage predominates the
desorption stage. The adsorption kinetic constant shows a
decreasing tendency with the raise in the resin/juice ratio, and the
desorption kinetic constant shows an increasing tendency. The
variation of the

I. Albert F. Vctor G. Salvador G. Alfonso (*) Food


Technology Department, Universitat de Lleida, Av.
Rovira Roure 191, 25198 Lleida, Spain e-mail:
garvin@tecal.udl.cat
I. Albert
e-mail: aibarz@tecal.udl.cat
F. Vctor
e-mail: vfalguera@tecal.udl.cat
G. Salvador
e-mail: garza@tecal.udl.cat

Springer

CIELab color parameters (L*, a*, and b*) with the adsorption
time was studied, obtaining results that match the kinetic
adsorption model proposed.
Keywords Adsorption . Kinetics model . Discoloration . Resin.
Apple juice. Browning
Notation
A Absorbance (dimensionless)
A0 Initial absorbance (dimensionless)
C
Resin concentration in the juice (grams resin/gram
juice)
Z
Adsorption efficiency (%)
m
Adsorbate concentration on resin surface (grams
melanoidins/gram resin) S Adsorbate
concentration in the juice
(grams melanoidins/gram juice) m0 Maximum
concentration of adsorbate retained in the
juice (grams melanoidins/gram resin) Kads Equilibrium
adsorption constant (Langmuir model,
grams juice/gram resin) KF Equilibrium adsorption
constant (Freundlich model,
grams juice/gram resin) n
Constant of adsorption
equilibrium (Freundlich
model, dimensionless) t
Adsorption time (hours)
ka Kinetic constant of the adsorption stage (grams
juice/gram resin second) kd Kinetic constant of the
desorption stage (per second) K
Equilibrium constant of
dynamic adsorptiondesorption process (grams juice/gram resin) mm
Adsorbate concentration on resin surface in equilibrium
conditions (grams melanoidins/gram resin) L* CIELab
color parameter (dimensionless) a*
CIELab color parameter
(dimensionless)
b* CIELab color parameter (dimensionless) L0 Initial value
of CIELab L* parameter

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(dimensionless) L Value of CIELab L* parameter


when equilibrium is
reached (dimensionless) a
Parameter associated to
the discoloration speed
(per hour)

Introduction
Two of the most important stability problems during the
processing of fruit juices are browning and turbid appearance. In
the case of apple juices, the main reason for these changes is the
oxidation of polyphenolic substances (Constenla and Lozano
1995;Fernndez de Simn et al. 1992;Falguera et al. 2011).
Browning is one of the most important processes of
deterioration that occurs in fruit juices during processing and
storage (Toribio and Lozano 1984), and consists of the
appearance of colored reaction products. There are two kinds of
browning: enzymatic browning and non-enzymatic browning
(Shahidi and Naczk 1995). Enzymatic browning is caused by the
action of polyphenol oxidase over phenolic substrates, resulting
in melanins. Non-enzymatic browning is caused by the reaction
between the reducing sugars and the free amino acids that result
in melanoidins. Both melanins and melanoidins are colored
products that confer the juice a dark color.
Different methods are currently used to reduce browning and
the possible turbidity. Turbidity treatment usually takes place
prior to the pasteurization process, and its utility is not to avoid
browning but to allow the reduction of colored compounds
(melanins and/or melanoidins) once they have been undesirably
produced during storage and/or thermal treatment. One of the
methods used to remove the color of juices is flocculation and
later sedimentation through the use of gelatine and bentonite
(Gokmen et al. 2001). This method has the disadvantage of
obstructing the pores of the membranes used in the clarification
stage. A method also used in the clarification of apple juices by
ultrafiltration is adsorption through polyvinylpolypyrrolidone
(PVPP; Gokmen et al. 2001;Humset al. 1980), but PVPP has the
inconvenience of being expensive and hard to recover. Another
method that can be used is the photochemical destruction of
these compounds (Ibarz et al. 2005), although it is expensive
and the products of the reaction are not known and could be
toxic. The adsorption method with cheaper and easier-to-recover
adsorbents is an alternative to remove the colored compounds
causing the turbidity that appears in juices (Carabasa et al. 1998;
Fisher and Hofsommer 1992; Qiu et al. 2007). The adsorbent
that meets these requirements is activated carbon, and it is
widely used with good results. If its particle size is very small, it
makes it hard to remove and able to contaminate the juice. If the
size is bigger, the price is much higher. There are other

adsorbent materials such as zeolites (natural and synthetic),


clays, silica gel, exchange resins, activated alumina, and some
synthetic polymers.
Lewatit S 4528 (Lanxess Energizing Chemistry, Edition
2009-11-19; www.lewatit.com) is a food grade resin and weak
basic macroporous anion exchange resin (tertiary and very low
level of quaternary amino groups) based on polystyrene.
According to the manufacturer's specifications, it is suitable in
the free base form for the decolorization of organic products
(colorants) such as fruit concentrates. The manufacturer
proposed this research because this resin has not been studied
before as an adsorption resin for decoloring.
Although the adsorption of dark-colored compounds in apple
juice has been studied by several authors (i.e., Gokmen and
Serpen 2002; Ataf and Gokmen 2011), the aim of this research
was to study the elimination of color compounds (melanoidins)
when they have been undesirably produced during the browning
reaction of apple juice with a new adsorbent Lewatit S 4528.
For that purpose, isotherms of the adsorption equilibrium at
different temperatures were obtained and adjusted to the
Langmuir and Freundlich models. The adsorption efficacy
according to the resin concentration, the adsorption kinetics, and
the evolution of color parameters (L*, a*, and b*) with time for
different resin/juice ratios were also evaluated.

Material and Methods


The sample of concentrated apple juice used in this study was
provided by an industry near Lleida (Spain) from the most
prevalent apple varieties (Starking Delicious, Golden Delicious,
and Granny Smith) processed in the Lleida region. This sample
was obtained from apples after the processes of selection,
cleaning, massing, pressing, depecti-nization, clarification, and
concentration up to 65Bx through evaporation in a Unipektin
industrial evaporator (Unipektin AG, Eschenz, Czech Republic).
The soluble solid content was determined using a digital
refractometer Atago RX-1000 (Atago Co. Ltd., Tokyo, Japan).
The adsorbent resin used was the Lewatit S 4528 (Bayer
Chemicals AG, Leverkusen, Germany). Its physical data are:
beige opaque ball-shaped grains with a specific surface (BET)
of 25 m2/g, bead size between 0.4 and 1.25 mm, pore volume of
0.35 cm3/g, pore diameter between 10 and 70 nm, bulk density
of 0.62 g/mL, and grain density of 1.02 g/mL. The resin was
dried by storing in a vacuum oven at 60 C until constant
weight prior to use.
First of all, the samples of the concentrated juice were
thermally treated at 70 C in a laboratory stove for 24 h. This
thermal treatment produced non-enzymatic (Maillard)

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browning reactions (melanoidins) in the juice that, after being


treated, was stored in a fridge at 4 C for further usage. This
thermal treatment also produced the conversion of polyphenols to
colorless forms (Brouillard 1982; Beveridge et al. 1986). In this
way, melanoidin concentration was directly proportional to the
absorbance at 420 nm, as was prior studied by Martins and Van
Boekel (2003). The melanoidin content was obtained as the
absorbance variation, as Falguera et al. (2010) did with melanins.
Absorbance measures were taken in a Helios gamma
spectrophotometer (Thermo Fisher Scientific Inc., Waltham,
USA) at 420 nm.
Equilibrium Model
Adsorption consists of the separation of a substance from a phase
through its accumulation or concentration on the surface of the
adsorbing phase. This transference process takes place until the
conditions of dynamic equilibrium are reached, being then when
the solution concentration remains constant, although the
adsorption and desorption with equal rates still take place. The
adsorption isotherms describe the relations between the
equilibrium concentrations of the adsorbate in the adsorbing
phase (m) and in the fluid phase (S) at a fixed temperature. The
Langmuir and Freundlich models are the most widely used to
describe the relation between both concentrations.
If a single adsorbate is only retained on a molecular surface,
the Langmuir model can be described as follows (Langmuir
1918):
(1)
OTQ

1 + KadsS

where m0 is the maximum concentration of adsorption retained by


the adsorbent, Kads is the constant of adsorption equilibrium, and
S is the concentration of the adsorbate in the fluid phase. Both
parameters depend on the temperature and the adsorbateadsorbent system; thus, for a specific application at a fixed
temperature, both remain constant.
The Freundlich model is empirical and can be described with
the following power equation (Freundlich 1906):
(2)
m = kFSn
where kF and n are adsorption parameters that depend on the
temperature and the adsorbate-adsorbent system.
To evaluate the adsorption efficiency of the colored
compounds contained in a browned juice through resins, the
following equation can be used:
x 100
AQ - A
AQ

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(3)

where A0 is the initial absorbance value and A is the final


absorbance value corresponding to the equilibrium conditions.
The colored compounds' retained concentration in the resin
can be obtained from the following equation:
AQ - A C
m
(4)
where A0 is the initial absorbance value, A is the concentration
measure of colored compounds (melanins and melanoidins) in the
juice, and C is the resin concentration per juice unit, defined as
grams resin/gram juice.
From the equilibrium constant, thermodynamic parameters
such as Gibbs free energy (AG), enthalpy change (AH), and
entropy change (AS) for the adsorption process can be obtained
using the following equations (Gokmen and Serpen 2002):
(5)

AH
AS

ln Kads
R
AG =-RT ln K d
(Van't Hoff's equation)

(6)

a s

where Kads is the adsorption equilibrium constant, T is the


absolute temperature, and R is the universal gas constant.
From the concentrated and thermally treated juice, 12Bx
samples were obtained by dilution with distilled water.
The absorbance measure prior to the addition of resin provides
information on the initial content of melanoidins in the juice.
A preliminary study was carried out to determine the necessary
time to reach the dynamic equilibrium between the fluid phase
(juice) and the adsorbent (resin). For that purpose, the absorbance
was measured during 24 h for each of the resin-juice relation
studied.
A known quantity of resin in the range of 0.5-3.5 g was added
to 50 g of juice. In this way, several samples were obtained with a
resin concentration in the juice between 0.01 and 0.07 g
resin/gram juice. The recipients containing the juice and resin
were placed for 24 h in a Bunsen BTG 1620 thermostatic shaking
bath (Bunsen, Madrid, Spain) with a fixed working temperature,
with the aim of reaching the equilibrium conditions at that
temperature. Once the equilibrium conditions were reached, the
samples were filtered using porous cellulose nitrate membranes
(Whatman International Ltd., Maidstone, England) with a pore
diameter of 0.45 |um. Finally, the absorbance at 420 nm was
measured to obtain the content of melanins and melanoidins in the
juice (S). This process was carried out at temperatures of 20, 35,
and 50 C. All the experiments were done in triplicate.
Kinetic Model
To carry out a kinetic study of the adsorption process, it is
necessary to define a mechanism that allows obtaining a kinetic
equation that properly describes the adsorption process. One of
these models is based on considering the

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0,5 OC
0,400

0.CO3

Fig. 1 Evolution of adsorption efficiency (Z) with resin/juice ratios at different temperatures
process as two-staged, one of adsorption and another of
desorption, both of them being first-order kinetic stages
(Langmuir 1918). This model has the disadvantages that it is
necessary to know the equilibrium constant in order to calculate
the equation parameters and the desorption constant cannot be
measured independently. To work out this inconvenience, an
approximate geometric model has been developed (Kuan et al.
2000; Qiu et al. 2007)to calculate the two constants.
Ibarz et al. (2008) developed an equation to describe the
variation with time of the adsorbate contents (colored solute) in
the resin:

way, small values of a* and b* mean that the sample is less

For each resin/juice ratio, seven samples were prepared, one for
each time: 0.5, 1, 2, 3, 4, 5, and 6 h. After the corresponding time
of adsorption, these samples were filtered through a 0.45 -|j.m
membrane filter prior to the measurement of absorbance values at
420 nm and
and
measuringthe CIELabcolor parameters (L*
b*). In the CIELab color space, L* stands for luminance, a* is the
red-green axis, and b* corresponds to the blue-yellow axis. In this

a so

0,12

colored. The color parameters L*, a*,and b* were obtained with a


Macbeth Color Eye 3000 spectrophotometer (MacbethKollmorgen Int. Corp.,

a
60 50
-

u
C

20
0,200

0,300

Absorbante at 4Z0 nm
0,16
O50!C 3S*C

20K

O50S
C

35?C
X 20'C

0.100

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dm ~d7

(7)

,-ti-

0,06

where m is the adsorbate concentration on resin surface, t is the


time, ka is the kinetic constant of the adsorption stage, and kd is the
kinetic constant of the desorption stage.
This equation can be integrated with the boundary condition
that the initial concentration of colored compounds in the resin is
zero, obtaining the following equation:

15
OS0C
1,5

20

A35SC
X205C

3,5 3

m = K(1 - e-kdt)

For high values of t, in which the equilibrium has been


reached:

If 2,5
0'

....a::-**

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= K = '-f-; kfl = mikd

(9)

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0.5

whichshows thatthe rates ofthe two stages ofcolorcompound


liberation and retention are in dynamic equilibrium.
A fixed quantity of resin (0.5, 1.0, or 1.5 g) was placed in an
empty recipient. Subsequently, 50 g of browned juice was added
and the recipient was placed in a thermostatic bath with a constant
temperature of 35 C.

-4

-3,5

-3

-2,5

-2

-1,5

-1

-0,5

Fig. 2 a Colored compounds adsorption isotherms on adsorbent resin at


different temperatures. b Adsorption isotherms compared with the
linearized Langmuir model. c Adsorption isotherms compared with the
linearized Freundlich model

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Table 1 Parameters for Langmuir
and Freundlich isotherms

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Langmuir model

Freundlich model

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m m0
K

adsS

l+KBdBS

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-k?Sn

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T (C)
20 35 50

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mo

R2

KF

23.752.32

7.951.84

0.9834

27.653.93

0.430.08

0.9593

37.261.09

8.700.61

0.9988

46.495.04

0.460.06

0.9826

81.988.82

3.790.48

0.9836

86.2510.01

0.610.15

0.9470

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Neuburgh, NY, USA) and the Macbeth Optiview software, which


uses the curve corresponding to the light source D-75 and
observer of 10. All absorbance measurements for the adsorption
process were corrected with those of the control sample for each
corresponding time interval in order to exclude thermal effect on
the measured absorbances.

data processing. All the fittings and the estimates were calculated
at a 95% significant level. All experiments and analysis were
carried out in triplicate.
a 24-h time frame; thus, the 24-h period is adequate for this
experiment.
Adsorption Efficiency

Color Evolution
A consequence of melanoidin adsorption is the discoloration of
the juice. Thus, to know the adsorption kinetics, the evolution of
the L*, a*,and b* CIELab parameters can be studied. The
following equation is used for L* (Carabasa and Ibarz 2000; Ibarz
et al. 1999):
L

(10)
0 +

(L

l - L )(1-e
0

-at

where L0is the L* parameter at time 0, Lx is the L* parameter


once the equilibrium is reached, and a is a parameter associated
with the discoloration rate.
Statistical Analysis
The experimental results obtained were fitted to the mathematical
models by using the Statgraphics (version
Plus 5.1, STCSC Inc. Rockville, Md, USA) software for

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Figure 1 shows the variation in the adsorption efficiency (z) for


resin concentrations (C) at different temperatures. It can be
observed that the efficiency of the adsorption increases with
temperature between 20 and 35 C. When temperature rises, the
motion of the pigments in the juice increases. This behavior
favors the different adsorption stages (external transference and
diffusion inside the resin), making the adsorption of the colored
compounds on the surface and inside the resin favored. It was
also observed that the adsorption efficiency asymptotically
increases with the resin concentration, which is evident since a
rise in the resin concentration entails a rise in the adsorption
surface. Minimal temperature influence on adsorption efficiency
was observed with higher resin concentration in the juice; thus, at
a low resin concentration, the adsorption efficiency was
temperature-dependent. These results are consistent with the
studies on vinegar presented by Achaerandio et al. (2002), on
clarified peach juice by Carabasa et al. (1998), on peach juice by
Ibarz et al. (2008), and on detergent by Leyva-Ramos (1989).
Between 35 and 50 C, the adsorption efficiency is

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Fig. 3 Resin adsorption dynamic curves, at 35 C, for three different ratios resin/juice

Results and Discussion


The preliminary experiment conducted has shown that a dynamic
equilibrium between phases can be obtained with

Table 2 Thermodynamic parameters


T (C)

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ads

AG (kJ/mol)

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Table 3 Kinetic constants values
in an adsorption process for
different resin/juice ratios at 35 C

^ = ka - kdm $ m

= K(1 - e-kdt)

Ratio (g resin/ g
juice
0.01
0.02
0.03

k (a.u. g juice/ g resin h)


7.811.44
7.371.22
7.150.38

kd (h-1)
0.450.13
0.580.13
0.690.05

mi = K = kd/kd (g juice/g
resin)
17.351.81
12.710.74
10.360.20

R2
0.9868
0.9894
0.9987

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temperature-independent, as was found by Fischer and


Hofsommer (1992)and Kimetal. (1992).
The fact that temperature has little effect on adsorption
efficiency, along with the inconveniences related to raising the
temperature and the resin concentration (favoring the nonenzymatic browning, warming over-cost, and higher resin
consumption over-cost), suggests working with the lower
temperature and the lower resin concentration that allow
obtaining a juice according to a colorimetric level prior defined.
If a low color level was desired, the process should use
temperatures between 35 a n d 5 0 C .
Adsorption Isotherms
Figure 2 shows that for a fixed absorbance value, the m variable
rises with temperature. The reason is that, as it is known, the
temperature rise causes a viscosity reduction (Augusto et al.
2011) and, therefore, a diffusion acceleration of the colored
compounds in the juice is produced, improving the global
adsorption process.
Equilibrium data were adjusted according to the Langmuir and
Freundlich models, which are the most widely used in the case of
mono-compound systems in which the solute is kept in an only
molecular surface. Table 1 shows the parameters of the

Fig. 4 Evolution of lightness with time of adsorption

adjustments of the experimental data to the Langmuir and


Freundlich models, and Fig. 2 shows the fits. Figure 2 and the
coefficients of determination of the adjustments of the data with
the two adsorption isotherms reveal that the two models permit
properly describing the behavior of the adsorption isotherms.
In Table 1, it can be observed that the adsorption equilibrium
constant of the Langmuir model, Kads, decreases with the
temperature increase. A value of Kads higher than the unit shows
that the process is a favorable type adsorption (McCabe et al.
1993). It can also be observed that the maximum concentration of
the adsorbed solute per adsorbent weight unit, m0, increases with
temperature. With regard to the Freundlich model, the KF constant
increases with temperature; the n exponent also increases with
temperature, being <1 in all cases. The main difference between
the Langmuir and Freundlich models is that the Langmuir model
is obtained as a theoretical process with simultaneous adsorption
and desorption stages, both of them with first-order kinetics,
while the Freundlich model is totally empirical.
Thermodynamic Parameters
Table 2 shows the thermodynamic parameters obtained for the
adsorption process. The negative values of AG for all the
temperatures tested indicate the spontaneous nature of the
adsorption process, as was obtained by

Fig. 5 Correlation between lightness and adsorption (m)

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Table 4 Adjustment parameters of
L* evolution for different
resin/juice ratios at 35 C

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Ratio resin/juice (g resin/g juice)
0.01
0.02
0.03

L = L'a + (Li
89.690.42
89.370.66
90.350.76

" Li) (1-e-at) Li


94.240.60
94.680.43
95.140.43

R2

0.480.18
0.920.32
1.120.48

0.9901
0.9860
0.9778

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Gokmen and Serpen (2002). The increment in the A G values


with temperature indicates that the adsorption process is not
favored by an increase in temperature. The fact that the value of
AH is negative indicates the exothermic nature of the adsorption
process. The slightly negative value of AS shows the slightly
decreased randomness at the solid/solution interface during the
adsorption process.
Adsorption Kinetics

interphase surface also rises, and therefore the material


transference rate behaves in the same way.
Figure 6 shows the evolution o f the a* and b * parameters,
proving a loss of color because of the decrease of both
parameters. Initially, both values decrease, but from a certain time
(lower as the resin concentration gets higher), the a* parameter
almost does not change and only the b* parameter continues its
decrease. A higher resin/ juice ratio entails a higher reduction of
both parameters, especially for b*. The global process is a

Fig. 6 Evolution of color parameters a* and b * w i t h t i m e o f adsorption


reduction of the reddish colors.
Figure 3 shows the evolution of the concentration of the colored
compounds that are retained by the resin at a temperature of 35
C for different resin/juice ratios. It can be observed that the
pigment concentration in the solid phase (m) rises with resin/juice
contact time, reaching an asymptote that corresponds to the
equilibrium achievement, as occurs in mass transfer when the
driving force depends on the difference between the
concentration and the equilibrium concentration. After 6 h, the
variation of the parameters was meaningless. The experimental
data fitted Eq. 8. Table 3 shows the values obtained in the
adjustments. In all cases, it can be observed that the value of the
kinetic constant of the adsorption stage (k a) is higher than the
kinetic constant of the desorption stage (kd). This fact allows the
adsorption of the colored compounds in the solid structure of the
resin.
Figure 4 shows the evolution of the L* parameter. It can be
observed that this evolution follows asymptotic kinetics with
adsorption time, which is consistent with the evolution of the m
concentration in Fig. 3, in accordance with the fact that the
adsorption kinetics consists of two stages (adsorption and
desorption).
Figure 5 shows the correlation between L* and m, showing
that the greater the adsorption, the lighter the juice becomes.
Table 4 shows the adjustment parameters of the L* parameter
with Eq. 10. The initial parameter, L 0, is almost the same in all
cases; the equilibrium value, L m, is also very similar. Thus, the
total discoloration does not depend on the resin/juice relation in
the ratio of the studied concentrations. The value of the a *
parameter increases with the resin/juice mass ratio. This can be
caused by the fact that when raising the resin/juice ratio, the

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Conclusion
The adsorption efficacy does not clearly rise when temperature
increases and rises when the amount of resin used increases.
Considering the technical and economic disadvantages associated
with these optimal conditions, the most reasonable option is to
work with the lowest parameters for both of them that allow
obtaining the desired characteristics of juice coloring.
The adsorption process is spontaneous, exothermic, and not
favored by an increase in temperature.
The values of the kinetic constant of the adsorption stage are
higher than the ones of the desorption stage. Thus, the
concentrations of adsorbed colored compounds in the steady state
are high.
The evolution of the adsorbed concentration values (m)and the
L* parameter values follows an increasing exponential function,
in accordance with the observed adsorption kinetics. The greater
the adsorption, the lighter the juice becomes.
The evolution of the a* and b* parameters shows a color
reduction, which continued for the b* parameter but limited for
the a* parameter, which is globally appreciated as a reduction of
the reddish colors.

References
Achaerandio, I., Gell, C., & Lpez, F. (2002). Continuous vinegar
decolorization with exchange resins. Journal of Food Engineering,
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