Rev.
Chapingo selective gas permeability, favor a reduction
Ser.Hortic vol.14 no.3 Chapingo sep./dic. 2008
Edible film based on arabic
gum and carboximethyl
cellulose to preserve fruits in
modified atmosphere
Recubrimiento comestible basado en
goma arbiga y carboximetilcelulosa
para conservar frutas en atmsfera
modificada
S. ValleGuadarrama*, O. Lpez
Rivera, M. ReyesVigil, J. Castillo
Merino y A. SantosMoreno
Departamento de Ingeniera Agroindustrial,
Universidad Autnoma Chapingo. Carretera
MxicoTexcoco, Km. 38.5, Chapingo,
Estado de Mxico, C.P. 56230.
Abstract
The aim of this work was to develop an
edible film based on arabic gum (AG),
carboximethylcellulose (CMC) and glycerol
(GL) as plasticizer and assess its potential
for covering fruits to preserve them in a
modified atmosphere. We evaluated its
mechanical properties in terms of
impermeability and light transmission. In an
evolutionary design phase an approximate
formulation of the film was obtained. With
this basis, a range of concentrations for AG
(20 and 30%), CMC (0.25, 0.50 and 0.75%)
and GL (5, 10 and 15%) were defined to
characterize the material. The combination
of 30% AG, 0.25 to 0.50% CMC and 5 to
10% GL was adequate for use in fruit
preservation in modified atmosphere
systems. By changing concentration of AG,
CMC and GL O2 and CO2 permeabilities and
mechanical resistance could be regulated.
Transparency was more than 80%.
INTRODUCTION
The modified atmospheres represent an
option to increase the useful life of the
horticultural products. In its development
plastic covers are used such as
polyethylene, polypropylene, among others,
which due to their inherent properties of
in the availability of O2 and an increase of
CO2 in the surrounding environment of the
product, which it induces a reduction of the
latter's metabolic activity (Kader, 2002).
As an alternative to plastic films, coatings
based on carbohydrates, proteins and lipids
can be used, which due to their composition
allow them to be edible. These materials are
applied directly to the surface of the
products and become part of them (Bosquez
et al., 2000; Debeaufort et al., 2000). In
resemblance to plastics, they develop
selective gas permeation properties
(Amarante and Banks, 2001) and therefore
can potentially replace them. On the other
hand, there is a need to reduce the use of
non-biodegradable materials for packaging,
because they constitute an important
percentage in the accumulation of solid
waste (Risch, 2000), which has generated
an important trend to develop modified
atmosphere systems in these edible
coatings.
Edible coatings can be applied in intact fruits
(Daz-Sobac et al., 1996, Del-Valle et al.,
2005) and in minimally processed products
(Emmambux and Minaar, 2003). In any
case, the selection of the components of a
formulation can be due to different
motivations: if you want to reduce the
moisture loss of the product, it is
recommended to use a lipocolloid or, if you
want to control the flow of gases such as O2
or CO2, it is common use of hydrocolloids
(Debeaufort et al., 2000). A double purpose
is often required, so a balance of both types
of materials is desirable, suggesting the
selection of compounds that favor the
control of a hydrophilic-lipophilic balance
(BHL).
Gum arabic (GA) is an effective emulsifier
that has the characteristics of low viscosity,
good surface activity and ability to form a
protective film in an emulsion; This
produces films with the properties of a
hydrocolloid and can form stable emulsions
with most oils (Chanamai and McClements,
2001), which favors the control of BHL.
Carboxymethylcellulose (CMC) is a polymer
that forms a film upon solidification, acts as
a binder, thickener and stabilizer (Girard et
al., 2002); In addition, it produces
transparent materials, which is an important
quality in coatings, as it allows to maintain
the appearance of the products. The CMC
has been used as part of edible films to
successfully delay the ripening and
senescence process of mango fruits (Daz-
Sobac et al., 1996), however, there are no
reports with the use of gum arabic.
Therefore, the objective of the work was to
develop an edible coating based on gum
arabic (GA) and carboxymethylcellulose
(CMC), to assess its potential for use in
modified atmosphere systems, by
evaluating its mechanical properties, gas
barrier and of light transmission.
MATERIALS AND METHODS
Experimental material
The GA and the CMC were selected as
polymers, for their emulsifying properties
and for their low opacity properties,
respectively. As a plasticizer, glycerol (GL)
was selected.
General experimental description
The study was carried out in two stages.
The first corresponded to the evolutionary
design in which the exploration was carried
out to develop the film and observe its
appearance with different concentrations of
GA, CMC and GL, under the different
dissolution time and temperature conditions.
The second stage was characterization. An
experiment was designed with 18 films
obtained from the combination of two levels
of GA (20 and 30%), three levels of CMC
(0.25, 0.50 and 0.75%) and three levels of
GL (5, 10 and 15%), for evaluate the
exchange capacity of O2 and CO2, the
modulus of elasticity and the capacity of
light transmission. To avoid the aging of the
samples, three groups were formed that
included each of the 18 formulations. Group
two was prepared at the end of the group
one evaluation and group three was
prepared at the end of the group two
evaluation. Each mixture was prepared with
distilled water, heating up to 90 C and
stirring without additional heating for 30
min.
The dispersions were allowed to cool to
room temperature and from each one 10 ml
were taken and emptied into the lid of a
petri dish. All units were allowed to rest for
24 h on a level basis. This stage was
developed as a factorial arrangement 2 x 3
x 3, under a completely random design,
where each component represented a
factor. With the obtained data, the analysis
of variance and the tests comparing means
(Tukey 0.05) through the SAS program
(SAS Institute, Inc., 1989).
Response variables
Transmission of light. Rectangular samples
of 0.5 x 4.0 cm were prepared and placed in
cells of a Spectronic Milton Roy model
Genesys 5 (USA) equipment perpendicular
to the light path. In each test tube the
transmittance was evaluated (in
percentage) at a wavelength of 540 nm. A
blank cell was used as blank or control.
Permeability to O2 and CO2. Each film was
placed between two petri dishes, to form a
cell with two chambers separated by the
material, where the tightness was created
with the application of thermal silicone. The
cameras had a monitoring port and ports of
entry and exit to allow a gaseous flow. In
the upper chamber, called the target
reservoir (Dd), a flow of 100 ml min-1 of
N2 was applied for 30 min. In the lower
chamber, called the source reservoir (Df), a
similar treatment was applied, but with
normal air. A zero time (t = 0) 1 ml of high
purity CO2 (99.8%) in Df was injected five
readings began recording the concentration
of O2 and CO2 in Dd, approximately every
15 min until complete . The results were
fitted by regression to the equation (1)
(Banks and Nicholson, 2000), where k1 by
Equation (2) and k2 (equal jf ay - YJD, 0)
was defined was the asymptotic line to the
curve formed by Equation (1) (Valle-
Guadarrama et al., 2002):
where R is the ideal gas constant (8.314 Pa
m-3 mol-1 K-1); T is temperature ( C); left. A tensile stress was applied with a
V is the internal volume (m3) of Dd; Ad is
the area (m2) of the membrane that divides
both deposits; yjd, t is the concentration (in
percentage) of O2 or CO2 in Dd at time t
(s); yjd, 0 is the concentration (percentage)
of O2 or CO2 in the same deposit at time
zero (t = 0); yjf is the concentration (in
percentage) of O2 or CO2 in Df and Pj 'is
the permeance (mol s-1m-2 Pa-1; Banks
et al., 1995) Jof the test film to O2 or CO2,
whose value was obtained from Equation
(2). Additionally, the thickness was
measured and the permeability of the
coating was calculated (Pj in mol m s-
1m-2 Pa-1), multiplying the permeance by
said membrane thickness (Banks et al.,
1995).
The O2 and CO2 concentrations were
determined with a gas chromatograph
(Varian model 3400CX, USA) with
Chrompack capillary column type poraplot
Q, with thermal conductivity detector (TCD)
and flame ionization detector (FID).
Temperatures of 80, 150 and 170 C were
used in the column, injector and detectors,
respectively. The column operated at a
gauge pressure of 158.5 kPa.
The quantification of O2 was assisted with
calibration standards (Praxair de Mxico
S.A. de C.V.) in balances of (2.01% O2 -
97.99% N2) and (4.98% O2 - 4.98% CO2 -
90.04% N2). For the CO2, a typical curve
was constructed, with containers of 7 ml
capacity and the combination of air with
CO2 (99.8%), to make mixtures of 0.03,
2.79, 5.54, 8.29, 10.48, 12.18 and 14.75%.
In all cases, samples were injected into the
chromatograph with glass syringes for gases
(Hamilton) in aliquots of 100 ml.
Resistance to tension. Test specimens were
formed with 6.0 cm high and 3.0 cm wide,
with a center perforation 0.6 cm in diameter
to induce a rupture point. The area of the
cross section in the central region varied
between 5.76 x 106 and 1.06 x 105 m2,
which was obtained with the product width
(2.4 cm) and thickness (262 8 m). The
specimens were clamped from the ends and
a free length between clamps of 4.0 cm was
texture analyzer equipment (TA-X2i, Stable
Micro Systems, UK) with a test speed of
0.001 m s-1, until completing a 0.030 m
path, which could or could not produce a
rupture of the material. As the materials did
not show a straight line at the beginning of
the stress-strain curve, the modulus of
elasticity was approximated by means of a
secant modulus (Mangonon, 1999),
measuring the stress for a unit strain of 5%,
and the product of such an effort for this
deformation was taken as secant modulus of
elasticity (Pa).
RESULTS AND DISCUSSION
Evolutionary design stage
The preparation of films with 30% GA and
drying for 12 h resulted in a smooth, brittle
material, without flexibility, with an opaque
appearance and with whitish spots. A
second set of tests, based on three levels of
GA (10, 20 and 30%) and two of
temperature (60 and 90 C) showed that
there was solidification from 20%, although
with higher concentration of GA it was
difficult to manipulate the mixture and
incorporated air that was not eliminated
during the rest. Also, it was determined that
the times required to obtain a suitable
solution at 60 and 90 C were 60 and 30
min, respectively, however, it was found
that if the condition of 90 C was applied in
a sustained manner it could cause
caramelization. In all cases, opaque
materials of brittle consistency were
obtained. The opacity was not a desirable
characteristic due to the eventual alteration
of the appearance of the horticultural
product to be coated; In addition, a brittle
consistency does not allow the stability of
the polymer on the product.
In parallel, tests were carried out with CMC,
which formed completely translucent
materials. In order to preserve the
emulsifying potential of the GA and obtain
the transparency characteristics of the CMC,
mixtures of both compounds were made.
When preparing a solution with 30% GA and
0.5% CMC, heating at 90 C and
subsequent mixing for 30 min, a translucent
material with a slight yellow tone was
obtained, without whitish spots, smooth,
bright and of brittle consistency. Finally, the
consistency was improved with the choice of
glycerol as a plasticizer, so with 30% GA,
0.5% CMC, 15% GL, heating at 90 C,
subsequent mixing for 30 min, emptying
and resting for 24 h, He obtained a
translucent and flexible material.
According to Sothornvit and Krochta (2000),
the addition of glycerol to a formulation
reduces the intermolecular force along the
polymer chain and this results in an increase
in flexibility.
Stage of characterization of the film
Transmission of light. The films presented
average light transmission of 81%, which
denotes a high degree of transparency, but
there was no significant difference between
formulations (Table 1). In the stage of
evolutionary design it was found that the
addition of CMC caused the coating to cease
to be opaque and acquire a transparent
appearance and the data in Table 1 suggest
that it is sufficient to add 0.25% of CMC in
the formulation to achieve this
characteristic. Currently there are no
quantitative reports on the degree of
transparency of other materials, which
prevents a comparison, however, the values
obtained in this work suggest that the
application of GA-CMC-GL coatings can be
done without altering the visual
characteristics of the horticultural products.
Secant module of elasticity. The results
showed that increasing the concentration of
GA required greater effort to deform the
films and therefore became more rigid and
less extensible (Table 1). However, the
factors of CMC and GL produced an opposite
effect, obtaining more extensible films with
the increase of concentration of these
compounds. The values found were of the
same order of magnitude as those reported
by Chick and Ustunol (1998) for different
films made with proteins. These authors
determined slightly higher values with
casein films, although the difference could
be due to the use of a probe displacement
speed of 50.8 cm min-1 in the stretch,
which was greater than that used in the
present work.
When a product is packaged, control is
sought over the exchange of gases with the
surrounding medium and protection against
mechanical stress during transportation,
packing and storage (Debeaufort et al.,
2000). The phenomenon of friction or
friction between fruits or against the walls of
the container, by effects of vibration during
the packaging or transport, is a factor that
accelerates the deterioration of a fruit.
Zamora-Magdaleno et al. (1999) evaluated
that the problem of friction in avocado fruits
can occur naturally, even before harvest
and that it is a function of the type of
management, so that the passage of the
product through the packer can cause
between 7 and 62% of it can not be
marketed, since fruits with higher symptoms
of friction at the end of the process show
higher rates of softening, so they suggested
the need to apply treatments to delay said
loss of firmness and provide protection
against of additional mechanical stress. In
fact, by inducing a modified atmosphere at
the tissue level with the use of a cover, a
delay in the loss of firmness of the product
is achieved, as demonstrated by Del-Valle et
al. (2005) with the application of a coating
based on cactus mucilage on strawberry
fruits, which translates into greater capacity
to maintain integrity against impacts and
friction. In the same sense, the application
of a coating helps in a situation of friction,
that does not act on the pericarp of the fruit
and decreases the damage. Amarante et al.
(2001), achieved within a packing unit the
decrease of the problem of discoloration
caused by the friction between pear fruits
with the use of a coating prepared with
carnauba wax.
To comply with a mechanical protection
objective, the coating must have a certain
capacity for deformation, such that when
exposed to an effort, the outermost layers
deform and leave intact those more internal
that contact the epidermis of the product.
Similar to the phenomenon of fluid flow in a
pipeline (Bird et al., 1960). The statistical
analysis reported that the mechanical
strength of the coating depends on a
significant interaction between the
components of the formula (Table 1). The
evaluation of this interaction confirmed that
the highest resistance is obtained with
higher GA content, but can be modulated in
a wide range with the addition of CMC and
GL in the ranges from 0.25 to 0.5% and
from 5 to 10%, respectively (Figures 1A, 1B
and 1C). This fact indicates that it is
convenient to select a high concentration of
GA and depending on the needs of the
product, the appropriate level of CMC and
GL should be selected, in order to obtain an
adequate coating resistance. However, other
aspects must be considered, which in a
combined way aim to improve the selection.
FIGURE 1: Effects of the interaction between
components of the formulations used in the
preparation of the coatings. Boxes A, D and
G explain the GAxCMC interaction, B, E and
H interaction GAxGL and C, F and I
interaction GLxCMC. Equal capital letters
indicate non-significant difference between
lines for the corresponding condition on the
abscissa axis. Equal lowercase letters
indicate non-significant difference to the
interior of each line (Tukey, 0.05) The bars
represent standard error (n = 3)
Permeability to O2 and CO2. Table 1
shows the values of permeability to O2 (O2)
and CO2 (CO2) obtained. No significant
difference was found between the levels of
the evaluated factors; however, a significant
interaction between them was found, which
indicated that the effect caused by any of
the components (GA, CMC or GL) depends
on the presence of the others.
For O2, the effect of changing concentration
of CMC with GA at 20% was different from
that caused with GA at 30% (Figure 1). With
GA at 20% there was a non-significant
increase when the CMC increased from 0.25
to 0.50%, but when varying from 0.50 to
0.75% the permeability to O2 was
significantly reduced. In contrast, with GA at
30%, it did not change when the CMC
changed from 0.25 to 0.50% and the value
exhibited was lower (P0.05) than with GA
at 20%. However, the passage from 0.50 to
0.75% generated an increase in the
exchange capacity of O2, to the extent that
the condition with 30% of GA the coating
became more permeable than with 20% of
the rubber (Figure 1D). The interaction
between GA and GL caused a reverse
situation (Figure 1E). With GA at 20%, the
increase in GL caused an increase in
permeability to O2 and with GA at 30% the
opposite effect was had. In this case, with
GL at low concentration the coating was
more permeable the higher the
concentration of GA; however, with high
concentrations of GL the highest
permeability was obtained with lower
GA. On the other hand, the evaluation of
the interaction between GL and CMC (Figure
1F) showed that with low concentration of
GL (5%) the behavior was similar to the GA
case at 30% when the amount of CMC was
increased, but with higher concentrations of
GL, the increase in CMC caused a behavior
of the type shown for GA at 20% (Figure
1D).
In the case of CO2, the result of the
interactions was a reverse behavior to that
described for the O2 permeability. With GA
at 20% the increase in CMC caused a
reduction in the CO2 exchange capacity, but
with GA at 30% an increase was induced
(Figure 1G). With GA at 20% the increase in
GL caused a reduction in CO2 permeability,
but with GA at 30% the result was also an
increase (Figure 1H). Finally, in the GL-CMC
interaction, it was found that with a low
concentration of GL (5%) the increase in
CMC caused the reduction of CO2, but when
GL was set at 10 and 15%, the increase in
CMC caused the increase in said
permeability or remained constant,
respectively (Figure 1I).
The permeation process consists of a
combined phenomenon of the solution of
the gas in the polymer and the transport
through it by diffusion (Kester and
Fennema, 1986).The presence of
interactions indicates that changing the
proportion of the components of the
formulations altered these mechanisms, but
a more detailed explanation will require that
in later works the structural change of the
formed polymer be explored.
On average, the materials were more
permeable to O2 (20.15 x 10-14 3.87 x
10-14 mol m s-1 m-2 Pa-1) than to 'Hass' avocado fruits in the manner
CO2 (7.56 x 10-14 1.83 x 10-14 mol m indicated. It is also applicable to lettuce,
s-1 m-2 Pa-1).
Likewise, the comparison with other
materials allows the classification of high
permeability to O2 and CO2 to coatings of
GA-CMC-GL, because Arvanitoyannis et
al.(1998) reported lower permeability values
(mol m s-1 m-2 Pa-1) in chitosa-
nogelatine-sorbitol films (O2: 2.593 x 10-
16, CO2: 1.12x10-15; M s-1 m-2 Pa-
1), (starch-hydroxyprolyl) -gelatin-glycerol
(O2: 4.8 x 10-15, CO2: 2.24 x 10-14),
(starch-hydroxyprolyl) -gelatin -sorbitol
(O2: 1.28 x 10-14, CO2: 7.04 x 10-14) and
(starch-hydroxyprolyl) -gelatin-sucrose (O2:
4.48 x 10-15, CO2: 1.60 x 10-
14). Jangchud and Chinnan (1999) reported
that peanut concentrate films exhibit O2
permeability of 3.68 x 10-18 mol m s-1
m-2 Pa-1, while McHugh and Krochta
(1994) found that the transmission of this
gas in protein materials isolated from whey
and glycerol occurs between 6.85 x 10-18
and 2.81 x 10-18 mol m s-1 m-2 Pa-1,
which is also lowerto the one found in the
present work. The comparison with plastic
materials confirms the greater permeation
capacity of GA-CMC-GL films, since
Cameron et al. (1995) pointed out that the
values, in mol m s-1 m-2 Pa-1, for low
density polyethylene are 2.7 x 10-15 for O2
and 9.9 x 10-15 for CO2; in the case of
polypropylene they reported 9.0 x 10-16 for
O2 and 5.8 x 10-15 for CO2 and in polyvinyl
chloride 1.9 x 10-17 for O2 and 6.5 x 10-17
for CO2.
Valle-Guadarrama et al. (2005), reported
that the minimum O2 permeance that
should exhibit a coating to preserve 'Hass'
preclimatory fruits was 1,963 x 10-10 mol
s-1 m-2 Pa-1. If the permeability is
divided by the thickness of the membrane,
the permeance is obtained (Banks et al.,
1995). The materials of GA-CMC-GL of the
present work had average values of
thickness and permeance equal to 262 m
and 7.69 x 10-10 mol s-1 m-2 Pa-1,
respectively. This indicates that such
materials could be used as coatings for the
since Cameron et al. (1995) suggested that
this product could be handled in a modified
atmosphere if a polyethylene film with a
permeance of 1.08 x 10-10 mol s-1 m-2
Pa-1 is used.
Coating selection
When a coating is applied on a product, the
gas exchange capacity of the product with
its immediate environment is reduced. As
the O2 intake required for the respiration
and the discharge of the CO2 generated in it
occur at a lower speed, a reduction of the
O2 concentration and an increase in CO2
inside the product itself is caused. After a
certain time, the rates of O2 consumption
and CO2 production are equalized with the
exchange rates through the shell-coating set
and constant concentrations are reached,
which is called a steady-state state
(Cameron et al. , nineteen ninety five). It is
essential to avoid O2 and CO2 being
installed at a lower or higher level,
respectively, than the tolerance limits of the
product, so when selecting a coating,
priority must be given to this criterion and
this involves defining the adequate values of
permeability to O2 and CO2 thereof.
The results of the present work show that it
is feasible to control the gas permeability of
the GA-CMC-GL coating, through the
concentrations of these components. If the
variables of light transmission and
mechanical resistance are considered, it is
convenient to choose a formulation based
on 30% GA and modulate the permeability
to O2 and CO2 by fixing the concentrations
of CMC and GL in the ranges of 0.25 to 0.5
and 5 to 10%, respectively, based on the
behavior shown in Figure 1.
It must additionally be considered that the
formulated material presents characteristics
of a hydrocolloid. In fact, it was observed
that the presence of high relative humidity
induced longer solidification times and sticky
tactile appearance in already formed
materials, which is attributed to the
hygroscopic properties of CMC and GL. It is
suggested, therefore, to explore the
hydrophilic-lipophilic balance (BHL)
management in later works, although this
could affect the gaseous exchange capacity
of the film, as shown by Ayranci and Tunc
(2001), who evaluated the effect of the
incorporation of fatty acids to control BHL in
a methylcellulose material and observed
that the gas exchange capacity decreased.
CONCLUSIONS
An edible film based on gum arabic (GA),
carboxymethylcellulose (CMC) and glycerol
(GL) was developed. The combination of GA
in proportion of 30%, CMC in a range of
0.25 to 0.50% and GL in a range of 5 to
10%, presented an adequate potential for
use in fruit conservation by modified
atmosphere systems. The change of
concentrations in GA, CMC and GL allows to
regulate the permeabilities to O2 and CO2,
modify their mechanical properties and
obtain light transmission capacity greater
than 80%.
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