Moisture adsorption characteristics of gingerbread, a traditional

bakery product in Pardubice, Czech Republic

L. Cervenka
*
, S. Rezkova, J. Kralovsky
Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, Nam. Cs. Legii 565, 532 10 Pardubice, Czech Republic
Received 31 January 2007; received in revised form 16 July 2007; accepted 20 July 2007
Available online 2 August 2007
Abstract
Adsorption isotherms of gingerbreads were obtained in the temperature range of 2030 C. The adsorption curves exhibited sigmoid
shape of to the type III isotherm, typical for many foods. Generally, increasing temperature decreased adsorbed moisture (negative tem-
perature eect) at low water activities, particularly in the curve for 20 C. However, the negative temperature eect was reversed above
water activity of 0.80 implying higher equilibrium moisture content at higher temperature. This altered temperature dependence of equi-
librium moisture content in relation to a
w
could be attributed to the presence of sugars. Of the four sorption models, the GAB model
gave the best t at all the three temperatures. Monolayer moisture and other properties of sorbed water were also obtained showing the
negative eect with increase in temperature. Isosteric heat of sorption obtained by applying ClausiusClapeyron equation decreased
exponentially with increasing moisture content. It could be implied from the results that keeping the moisture content of gingerbreads
below 1215% d.b. (equivalent to 6064% of relative humidity) may ensure long shelf life of this products during storage at room
temperature.
2007 Elsevier Ltd. All rights reserved.
Keywords: Gingerbread; Adsorption isotherm; Heat of sorption
1. Introduction
The production of gingerbreads in the Czech Republic,
especially in Pardubice, has a long tradition since the Mid-
dle Ages. Gingerbread is a sweet bakery product that can
take the form of a cake or a cookie in which the predomi-
nant avor is ginger. Gingerbread can be made into a thin,
crisp cookie or a softer cookie cut into various shapes. The
formula for gingerbread dough may vary depending on
local custom. Generally, it comprises wheat our, sugar,
honey, condiments and chemical leavens. Honey can be
replaced by sucrose hydrolysate in the large-scale produc-
tion. This type of product belongs to the category of the
bakery products with long shelf-life stability, however it
was previously reported that gingerbreads were associated
with occurrence of xerophilic fungi (Vytrasova, Pribanova,
& Marvanova, 2002), which may cause deterioration of
these products under inappropriate storage conditions.
Knowledges of the moisture content and water activity
relationships of a food product are very important. These
can be formulated by determining moisture sorption iso-
therm which can be used for dening storage conditions,
and in making shelf life determination (Mathlouthi,
2001). Despite its long tradition, the moisture adsorption
behavior of gingerbread has never been published (to the
authors knowledge).
Many empirical relations describing the sorption char-
acteristics of foods or food ingredients have been pro-
posed in the literature (Al-Muhtaseb, McMinn, &
Magee, 2002). The equations usually applied for the food
systems are GAB (Samaniego-Esguerra, Boag, & Robert-
son, 1991) and BET (Brunauer, Emmet, & Teller, 1938)
equations. The monolayer moisture content, a key
parameter corresponding to the physical and chemical
0260-8774/$ - see front matter 2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jfoodeng.2007.07.006
*
Corresponding author. Tel.: +420 466 037 718; fax: +420 466 037 068.
E-mail address: libor.cervenka@upce.cz (L. Cervenka).
www.elsevier.com/locate/jfoodeng
Journal of Food Engineering 84 (2008) 601607
stability of foods, could be derived using these models.
However, the applicability of the BET model is limited
because it has proved to t water sorption data only
over the narrow a
w
range from 0.1 to 0.5 (Al-Muhtaseb
et al., 2002). The GAB model primarily derived from the
BET model has been shown to t experimental sorption
data for almost all food materials and cover the whole
a
w
range. This feature makes the GAB model to be ver-
satile sorption model. In addition, dierent properties of
sorbed water can be obtained by tting the Caurie equa-
tion (Caurie, 1981) or Henderson equation (Igbeka &
Blaisdell, 1982).
The objective of the present study was to establish the
equilibrium moisture content and water activity data for
gingerbread at dierent temperatures so as to analyze them
with dierent models and generate moisture sorption
parameters as well as other properties of sorbed water,
and evaluate the isosteric heat of sorption.
2. Materials and methods
2.1. Preparation of samples
Four gingerbread samples (softer cookies of various
shapes) were purchased from four local bakers in Pardub-
ice, Eastern Bohemia. The samples were packed in various
packaging materials (polyethylene, cellophane). Since dif-
ferent bakers prepared the gingerbreads and each has its
own recipe, the dierences were in shape, taste, consistency
and in color. However, none of these dierences have been
experimentally evaluated. According to our un-published
results, the main variability among gingerbread samples
was the fat content and simple sugar composition
(Cervenka et al., 2007). The proximate composition of
the masterbatch was described with calculated mean values
(Table 1). The masterbatch was prepared from equal
amount of each gingerbread sample by manual grinding
in mortar. Thereafter, the milled sample was sieved to give
particles size of <1.0 mm. The mixture was pre-dried in
forced-air oven at 50 C for 24 h, and subsequently dried
over silica gel in a desiccator at room temperature until
weight constancy. Then, it was kept over dried silica gel
until used in the experiment.
2.2. Moisture adsorption isotherms
For sorption studies the following salt slurries were used
(Stolo, 1978): lithium chloride, potassium acetate, magne-
sium chloride, potassium carbonate, magnesium nitrate,
cobalt chloride, strontium chloride, sodium chloride,
ammonium sulphate, potassium chloride and barium
chloride.
Novasina A
w
Sprint (TH 500, Axair Ltd., Switzerland)
instrument was used for detecting that equilibrium has
been reached. The sample (approximately 1 g) was depos-
ited above the selected saturated salt slurries at 20, 25
and 30 0.2 C to attain equilibrium. The equilibrium
was reached when values of a
w
and temperature did not
change by more than 0.001 a
w
and 0.1 C after three con-
secutive 10 min intervals. The humidity sensor is based
on conductivity changes in a hygroscopic electrolyte. The
equilibration time, however, depends on the a
w
level;
approximately 4 h in the range of 0.1130.45, 8 h in
Table 1
Proximate chemical composition of gingerbread masterbatch (Cervenka
et al., 2007)
Constituent Mean value
a
(g/100 g) Variability (g/100 g)
Ash 0.75 (0.501.20)
Moisture 7.53 (5.209.30)
Protein 8.08 (7.608.60)
Fat 3.25 (1.107.00)
Sucrose 19.70 (2.2035.90)
Fructose 5.80 (2.807.80)
Glucose 6.97 (4.0012.50)
Total carbohydrate 79.45 (77.9383.26)
a
Calculated according to data of Cervenka et al., 2007.
Nomenclature
A surface area of sorption (m
2
g
1
)
a
w
water activity
C density of bound water (g ml
1
)
C
1
constant related to heat of sorption in BET
equation
C
2
, K constants related respectively to monolayer and
multilayer properties of water in GAB equation
E mean relative deviation (%)
H
1
heat of condensation of pure water vapor
(kJ mol
1
)
H
m
heat of sorption of the rst layer (kJ mol
1
)
H
n
heat of sorption of a multilayer (kJ mol
1
)
m moisture content (% dry basis)
M

0
, C

2
, K
*
pre-exponential factors
M
0
monolayer moisture content (% dry basis)
N number of monolayers
n number of observation
n
1
, k constants of Henderson equation
Q
st
net isosteric heat of adsorption (kJ mol
1
)
R ideal gas constant = 8.314 (J mol
1
K
1
)
R
2
coecient of regression
S slope of Cauries plot
T absolute temperature (K)
DH Arrhenius type energy factor (kJ mol
1
)
Subscripts
e experimental
p predicted
602 L. Cervenka et al. / Journal of Food Engineering 84 (2008) 601607
0.450.75 and 12 h at very high a
w
levels (i.e. 0.750.90).
The rate of approach to equilibrium in a chamber is also
function of various parameters; these include the physical
nature of the gingerbread, the specic surface area and
transport conditions in the air space above the sample.
The relatively rapid equilibration time of Novasina instru-
ment may be attributed to small headspace in the sample
container (Kitic, Favetto, Chirife, & Resnik, 1986).
The samples were weighed on analytical balance (sensi-
tivity 0.001 g) after the equilibrium had been attained.
The adsorption isotherms were obtained by plotting the
moisture content of the samples, expressed as percentage
of moisture on dry basis versus a
w
. Each isotherm was con-
structed using data of three consecutive measurements.
2.3. Isotherm models
The equilibrium moisture data were tted using the
equations in their linear form:
BET:
a
w
m1 a
w

1
M
0
C
1

C
1
1a
w
M
0
C
1
1
Caurie:
ln
1
m
lnCM
0

2C
M
0
ln
1 a
w
a
w
2
The number of adsorbed monolayers (N) was calculated
using the formulae (Caurie, 1981):
S
54:45
A
3
N
2
S
4
where A is the surface area (m
2
g
1
) and S is the slope of
Cauries plot. The M
0
values were evaluated using the
BET plot with a
w
up to 0.65 against a
w
/m(1 a
w
) and
using Cauries plot of ln(1 a
w
)/a
w
versus ln1/m in the
a
w
range from 0.1 to 0.8.
The GAB equation was rearranged into a second degree
polynomial equation in the range of 0.10.9 a
w
(Samani-
ego-Esguerra et al., 1991)
a
w
m
aa
2
w
ba
w
c 5
where
a
K
M
0
1
C
2
1

6
b
1
M
0
1
2
C
2

7
c
1
M
0
C
2
K
8
In addition, the inuence of temperature on GAB con-
stants may be calculated with an Arrhenius form of equa-
tion (Sanni, Atere, & Kuye, 1997). That is:
M
0
T M

0
expDH=RT 9
C
2
T C

2
expH
m
H
n
=RT 10
KT K

expH
l
H
m
=RT 11
where M

0
, C

2
and K
*
are pre-exponential factors; H
m
, H
n
and H
l
are the molar sorption enthalpies of the monolayer,
multilayers and bulk liquid, respectively. Similarly, the iso-
therms were analyzed using the Henderson equation in the
linear form (Igbeka & Blaisdell, 1982)
Logln1 a
w
n
1
Logm Logk 12
Using a
w
values up to 0.9, the constants (n and k) were
computed by the least squares method. The goodness of
t of the models was evaluated with the mean relative devi-
ation (%E) between the experimental and predicted mois-
ture contents in the modied formula:
%E
100
n
X
m
e
m
p
m
e

13
The net isosteric heats of adsorption (Q
st
) were calculated
from the following form of ClausiusClapeyron equation
applied at two temperatures, T
1
and T
2
.
Q
st
R
T
1
T
2
T
2
T
1

ln
a
w2
a
w1

14
where a
w1
and a
w2
are water activities at absolute temper-
atures T
1
and T
2
, respectively (Kumar, Singh, Patil, & Pa-
tel, 2005).
3. Results and discussion
3.1. Moisture adsorption isotherms
The results of the experimental measurements of the
equilibrium moisture contents of gingerbread sample at
20, 25 and 30 C are given in Fig. 1. These temperatures
were selected as possible storage conditions. The shape of
the isotherms at all temperatures is characteristic of high-
sugar-containing foods, which sorb relatively small amount
of water at low water activities and large amounts at high
Fig. 1. Experimental and predicted moisture sorption isotherms of
gingerbread using GAB equation at dierent temperatures.
L. Cervenka et al. / Journal of Food Engineering 84 (2008) 601607 603
water activities, particularly above 0.60 a
w
. Fig. 1 also
shows the eect of temperature on the sorption isotherms
of gingerbread sample. It can be seen that equilibrium
moisture content was generally higher at 20 C for a similar
water activity in comparison with those measured at 25 and
30 C. The isotherms obtained at 25 C and 30 C were
almost identical up to 0.70 a
w
and temperature eect was
negligible. The negative temperature eect on equilibrium
moisture content has been observed in many foods of
high-sugar content (Ertugay & Certel, 2000; Palou,
Lopez-Malo, & Argaiz, 1997; Turhan, Oymael, & Ekiz,
2003). The negative eect of temperature on the equilib-
rium moisture content at low water activities can be related
to the fact that, while polymers (starch or protein) sorb
more water than sugar and other soluble components at
low water activities, the soluble components such as sugar
sorb more water at higher water activities. Therefore the
negative temperature eect is eliminated at higher water
activities. This is consistent with other foods with high-
sugar content such as dried plantain slices (Falade, Ade-
tunji, & Aworh, 2003), Turkish tarhana powder (Ibanoglu,
Kaya, & Kaya, 1999), African mango (Falade & Aworh,
2004) or rice based milk desert kheer (Kumar et al.,
2005). On the other hand, the crossing of the isotherms
has not been observed in cookies and corn snacks (Palou
et al., 1997) or various cereals (Ertugay & Certel, 2000)
which contain mainly complex carbohydrates rather than
simple sugars.
3.2. Isotherm models
Four isotherm equations (Eqs. (1), (2), (5), (9)) were
used for establishing the degree of t to experimental data.
Estimated parameters for these models have been presented
in Table 2. In gingerbread sample, two of the equations t-
ted to the adsorption data in the range of a
w
0.1130.892,
GAB and Caurie equations, exhibited low %E values. It
was previously published that these two equations were
the best to characterize sorption behavior of most foods,
like cereals, maize or various milk products (Caurie,
1970; Hossain, Pal, Sarkar, & Patil, 2002; Kumar et al.,
2005). The BET equation yielded low mean relative devia-
tion as well (%E < 1.5) but its applicability was limited up
to 0.600.65 a
w
depending on the temperature used in the
present study. Upward curvature of BET plot above
0.600.65 a
w
has been observed. The BET isotherm can sat-
isfactorily model sorption in the range of a
w
from 0 to 0.45
(Al-Muhtaseb et al., 2002; Arogba, 1999; Marcos et al.,
1997). It has been shown that, at higher water activities,
less gas or vapor is sorbed than indicated by the BET equa-
tion causing the upward curvature of the BET plots (Tim-
mermann, 2003). Henderson equation gave relatively
higher %E values at all temperatures in comparison to
BET and GAB equations.
3.3. Properties of sorbed water
The physical state of the water in foods determines the
spoilage (Ross, 2001). It is therefore suitable to generate
information related to various aspects of bound water
viz., its density, its relation to surface area of sorption of
adsorbent, number of absorbed monolayers, etc.
The monolayer moisture contents of gingerbread mix-
ture at each temperature were calculated using GAB and
BET equations and are presented in Table 3. The mono-
layer moisture calculated from GAB equation (6.38
7.31% d.b.) was higher than those obtained from BET
equation (5.866.38% d.b.) and generally decreased with
increase in temperature of adsorption, as has been
observed in other food systems (Falade & Aworh, 2004;
Kumar et al., 2005; Palou et al., 1997; Samaniego-Esguerra
et al., 1991). According to Timmermann (2003), the GAB
constants have to be taken as being the representative
parameters of the multilayer sorption. The monolayer
moisture content of gingerbread was higher (6.38
7.31% d.b.) than those determined in similar foods after
temperature treatments (i.e. baking). For instance, Palou
et al. (1997) calculated the GABs monolayer moisture con-
Table 2
Estimated parameters for selected models of adsorption isotherm equations for gingerbread at dierent temperatures
Equation Temperature (C) a
w
Constants %E
a b c
GAB 20 0.1100.898 0.091 0.056 0.043 0.59
BET 0.1100.648 0.118 0.039 1.63
Caurie 0.1100.898 0.692 2.327 1.71
Henderson 0.1100.898 0.996 1.215 3.34
GAB 25 0.1130.894 0.099 0.052 0.054 0.85
BET 0.1130.631 0.120 0.051 1.44
Caurie 0.1130.631 0.729 2.203 1.39
Henderson 0.1130.631 0.971 1.132 3.14
GAB 30 0.1130.892 0.096 0.040 0.060 0.81
BET 0.1130.608 0.108 0.059 0.64
Caurie 0.1130.892 0.772 2.187 1.02
Henderson 0.1130.892 0.873 1.025 3.51
604 L. Cervenka et al. / Journal of Food Engineering 84 (2008) 601607
tent for various cookies to be 3.95.0% d.b. in the temper-
ature range from 25 C to 45 C. The same parameter var-
ied from 6.0 to 7.0% d.b. at 30 C for wheat our
(Riganakos, Demertzis, & Kontominas, 1994). With the
increase in temperature the number of adsorbed monolay-
ers and surface area of sorption decreased whereas density
of sorbed water did not show denite temperature depen-
dence for the range (2030 C) of temperatures studied
(Table 3). Increase in surface area exposes more charged
polar groups and carboxyl functions of peptide bond
enhancing the water sorption. The similar surface area of
sorption has been observed in kheer (7983 m
2
/g), a food
rich in sugars such as sucrose and lactose (Kumar et al.,
2005).
The temperature dependencies of the GAB constants
calculated using linear regression are shown in Table 4.
As was expected, more than one straight line could be
tted. According to hypothesis of Rockland (1969), the
Henderson isotherm should be, theoretically, divided into
three local isotherms, each corresponded with characteris-
tic types of bound water, i.e. monolayer, multilayer and
free water. Thus the breaks in the curves indicate changes
in the type of water binding. In our study, only one inter-
section point has been observed (Fig. 2) representing the
transition from multilayer sorbed water to mobile water
as with similar studies reported on other food items (Aro-
gba, 1999; Igbeka & Blaisdell, 1982; Lima & Cal-Vidal,
1983). In the present study, the isotherms intersected at
moisture content of 12.0% and 15.5% (on dry weight basis)
at 20 C and 30 C (Table 3). These moisture contents rep-
resent the highest or critical values at which the water mol-
ecules are bonded to other chemical groups. At higher
values of moisture content, the water is considered as
unbound, free water found in interstitial pores of food sam-
ple (Rockland, 1969). The gure also show shift to the left
with increase in temperature in lower water activities.
Extrapolated from Fig. 1, the corresponding water activi-
ties are in the range from 0.60 to 0.64 at temperature from
20 C to 30 C. At higher values of a
w
, the gingerbread may
deteriorate in quality.
3.4. Isosteric heat of sorption
As data did not show denite temperature dependence
for the range of temperature studied (2030 C), Eq. (11)
was used to obtained net isosteric heat of sorption by
considering 20 C and 30 C as T
1
and T
2
. The isosteric
heat is plotted in Fig. 3. The curve shows that the heat
Table 3
Properties of bound water of gingerbread at dierent temperatures
Temperature (C) Monolayer moisture (% d.b.) Density of sorbed
water, C (g/ml)
No. of adsorbed
monolayers, N
Surface area of
sorption, A (m
2
/g)
Henderson plot
BET GAB Breakpoint Moisture (% d.b.)
20 6.38 7.31 1.882 2.89 78.73 1.19 15.5
25 5.86 6.55 1.816 2.74 74.65 1.15 14.1
30 6.00 6.38 1.854 2.59 70.55 1.08 12.0
Table 4
Temperature dependencies of GAB constants for gingerbread
M
0
(T) C
2
(T) K(T)
M

0
DH R
2
C

2
H
m
H
n
R
2
K
*
H
l
H
n
R
2
0.113 10.136 0.896 2.5 10
3
17.560 0.991 3.078 2.923 0.680
Fig. 2. The Henderson plots of gingerbread at 20 C and 30 C.
Fig. 3. Net isosteric heat of sorption of gingerbread at temperatures
ranged from 20 C to 30 C.
L. Cervenka et al. / Journal of Food Engineering 84 (2008) 601607 605
of adsorption decreased with increase in moisture con-
tent, initially rapidly up to 15% d.b. and later slowly,
as observed in many other food systems (Aviara, Ajibola,
& Oni, 2004; Falade et al., 2003; Kaymak-Ertekin &
Gedik, 2004; Kumar et al., 2005; Turhan et al., 2003).
The decrease in the isosteric heat with the increase in
sorbed water content may be attributed to the fact that
sorption initially occurred in the most active sites giving
rise to the greatest interaction energy. With increase in
the moisture content these sites are occupied, then sorp-
tion occurs on the less active sites resulting in lower heats
of sorption. As the isosteric heat tends to zero, the inu-
ence of the adsorbent on the adsorbed molecules becomes
negligible, i.e. additional sorbed water molecules repre-
sent so-called free water available for microorganisms.
The equilibrium moisture content of gingerbread at
which isosteric heat of adsorption is close to zero (i.e.
15.0% d.b.) corresponded well to safe moisture content
derived from Henderson equation. Negative values of
heat of sorption at high moisture content are a direct
contribution of the endothermic dissolution of sugar in
the sorbed water (Falade et al., 2003; Kaymak-Ertekin
& Gedik, 2004). However, the negative Q
st
value has
no physical meanings and might be within the error of
mathematical determination (Kaymak-Ertekin & Gedik,
2004).
4. Conclusion
Moisture sorption isotherms of gingerbread obtained
for the temperature range of 2030 C were sigmoid type
III, common to most foods (Al-Muhtaseb et al., 2002). A
negative temperature eect was evident with regard to
the equilibrium moisture content, particularly in the
curve representing 20 C. However, the negative temper-
ature eect was reversed above water activity of 0.80.
This altered temperature dependence of equilibrium
moisture content in relation to a
w
could be attributed
to the presence of sugar. Sorption data were best
described by the GAB model. Monolayer moisture
obtained from GAB equation was higher than those
obtained from BET equation and decreased with increase
in temperature. Properties of sorbed water were obtained
to understand changes in the sorbed water caused by
change in temperature during storage. The net isosteric
heats of adsorption were obtained using ClausiusCla-
peyron equation. It could be implied from the results
that keeping the moisture content of gingerbreads below
1215% d.b. (equivalent to 6064% of relative humidity)
may ensure long shelf life of this products during storage
at room temperature.
Acknowledgement
Financial help for this project was provided by Ministry
of Education, Youth and Sports of the Czech Republic
(project No. 0021627502) and by the Grant Agency of
the Czech Republic (Project No. 203/05/2106).
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