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Original article
Desorption isotherms, net isosteric heat and the effect of
temperature and water activity on the antioxidant activity of two
varieties of onion (Allium cepa L)
Armand A. Bouba,1* Nicolas Y. Njintang,2,3 Gilles Bernard Nkouam,1 Yannick Dimitry Mang,4
Abul-Hamd El-Sayed Mehanni,5 Jo€el Scher,6 Didier Montet7 & Carl Moses Mbofung3
1 Department of Agriculture, Livestock and By-products, ISS, University of Maroua, PO Box 46, Maroua, Cameroon
2 Department of Biological Sciences, Faculty of Science, University of Ngaoundere, PO Box 454, Ngaoundere, Cameroon
3 Department of Food Science and Nutrition, ENSAI, University of Ngaoundere, PO Box 455, Ngaoundere, Cameroon
4 Department of Life and Earth Sciences, ENS, University of Maroua, PO Box 46, Maroua, Cameroon
5 Department of Food Science, Faculty of Agriculture, Sohag University, Sohag 82786, Egypt
6 Laboratory of Biomolecular Engineering, ENSAIA, INPL, Nancy-Universite, B.P. 172 F-54505 Vandoeuvre-Les-Nancy 2, Avenue for^et de
la Haye., Nancy, France
7 Cirad, UMR Qualisud, TA B95/16, Montpellier Cedex 5 34398, France
(Received 1 February 2013; Accepted in revised form 30 July 2013)
Summary The standard static gravimetric method was used to determine moisture desorption isotherms (MDIs) of
two onion varieties (Goudami and Galmi Violet) at 30 °C, 45 °C and 60 °C in the water activity ranging
from 0.055 to 0.83. The combined effects of temperature and water activity on the antioxidant activities
of the onion varieties were also studied. GAB, Oswin, Smith and BET equations were tested to fit the
experimental data. The net isosteric heat of sorption was calculated. Equilibrium moisture content
(EMC), total phenolic content (TPC) and antiradical activity were also measured. The isotherm and the
EMC vary significantly with the onion variety and drying temperature, irrespective of water activity (aw).
Desorption isotherms were best described by the GAB model. The maximum net isosteric heats for Galmi
Violet (32.58 kJ mol1) were greater than those of Goudami (23.50 kJ mol1) at each EMC. The TPC
and antiradical activity of the Galmi Violet were significantly (P ≤ 0.05) higher than that of the Goudami
at all investigated temperatures and water activities.
Keywords Allium cepa L., antioxidant activity, isosteric, isotherms.
doi:10.1111/ijfs.12321
© 2013 The Authors. International Journal of Food Science and Technology © 2013 Institute of Food Science and Technology
Desorption isotherms of two onion varieties A. A. Bouba et al. 445
© 2013 The Authors International Journal of Food Science and Technology 2014
International Journal of Food Science and Technology © 2013 Institute of Food Science and Technology
446 Desorption isotherms of two onion varieties A. A. Bouba et al.
as shown in Table S2. These equations were the most temperature for 2 h and filtering through Whatman
widely used to fit the experimental sorption data of No 1 (Maidstone, England) filter paper. Residues were
various food materials (Kaymak-Ertekin & Gedik, re-extracted with additional 25 mL of methanol for a
2004). Although GAB model was considered as an further 2 h and filtered as described. The volume of
extension of the BET model, it had a reliable theoreti- the combined extract was removed by evaporation,
cal base and parameters that described the effects of and the lot stored in a sealed tube at 4 °C until
temperature on the isotherms by means of the Arrhe- required for use.
nius-type equations (Rizvi, 1986). The parameter val-
ues of the tested models were estimated by nonlinear Ferric-reducing antioxidant power (FRAP)
regression with the experimental result using the soft- The antioxidant potential of the different onion
ware Sigma-plot11.0 (Systat software, Inc., San Jose, extracts was also evaluated by their ability to reduce
CA, USA). The best fitting equations (eqn 1) were iron (III) to iron (II) following the method of Chan
evaluated with the mean relative percentage deviation et al. (2009). In this respect, 1-mL aliquot of each
(P) and determination coefficient (R2), and P was extract, dissolved in distilled water, was mixed with
defined as follows: 2.5 mL of phosphate buffer (0.2 M, pH 6.6) and
N
2.5 mL of 1% aqueous KFe (CN) solution and incu-
100 X Mei Mpi bated for 30 min at 50 °C. After this, 2.5 mL of 10%
Pð%Þ ¼ ð1Þ
N i¼1 Mei TCA was added, and the mixture was centrifuged for
10 min. A known volume of 2.5-mL aliquot of the
where Mei and Mpi are the experimental and predicted supernatant was mixed with 2.5 mL of distilled water
moisture content values, respectively; N is the number and 0.5 mL of 0.1% aqueous FeCl3, and the absor-
of experimental data. This model was considered bance was recorded at 700 nm. Ferric-reducing
acceptable when P values were below 10% (Boquet antioxidant power was determined as ascorbic acid
et al., 1978). equivalents (mg ascorbic acid per g extract).
Calculation of the isosteric net heat of sorption Determination of total phenol content
Total phenol content was determined using the Fo-
The net isosteric heats of sorption were determined by lin–Ciocalteu colorimetric method as described by A-
the moisture desorption data using the classical marowicz et al. (2004). Plant extracts (20 lL) were
Clausius–Clapeyron’s equation (eqn 2). mixed in a test tube with 0.2 mL of Folin–Ciocalteu
This equation links the variation in pure water reagent and 2 mL of distilled water and incubated at
vapour partial pressure (P0) with T. room temperature for 3 min. Following this, 1 mL of
dLnP0 =dð1=TÞ ¼ k=R ð2Þ 20% sodium carbonate was added to the mixture and
reincubated for 2 h at room temperature. The absor-
That is, the net isosteric heat of sorption can be cal- bance of the resulting blue colour was measured
culated by plotting the sorption isostere. –lnaw = f(1/T) using a quartz curve at 765 nm. Gallic acid was used
for a specific moisture content of material and deter- as standard, and total phenols were expressed as
mining the slope that equals Qs/R. This procedure was gram gallic acid equivalents (GAEs) per 100 g of dry
repeated for different moisture contents to determine basis.
the dependence of Qs on the moisture content (Kapseu The ability of dried onion extracts to scavenge the
et al., 2006). DPPH radical was measured using the method of Sun
et al. (2005) with some modifications. In brief, 0.3 mL
of radical DPPH 10 mM solution, 2.4 mL of ethanol
Analysis of antioxidant activity
at 99% and 0.3 mL of the sample extract were mixed
Onions obtained after desorption by the static gravi- rigorously and quickly. The scavenging capacity was
metric method were ground and used in the extraction evaluated by spectrophotometry at 517 nm. The per-
of antioxidants. Efficiency of extraction is an impor- centage of inhibition was calculated using the follow-
tant factor for the comparison of antioxidant activity. ing equation:
Previous studies reported that relatively higher antioxi- DPPH ð%Þ ¼ ½ðODcontrol ODassay Þ=ðODcontrol Þ 100
dant activities were observed from methanolic extracts
in onion varieties (Abdou Bouba et al., 2012). For this A calibration curve of percentage inhibition versus
reason, methanol was selected as the solvent of choice quercetin concentration was plotted using quercetin
for extraction in this study. The methanolic extracts standard solutions (2.0 mM, 1.25 mM, 1.0 mM,
were obtained from 20 mg mL1 of ground spice sam- 0.75 mM, 0.50 mM). Based on the calibration curve,
ple. In brief, 250 mg of ground spice sample was the DPPH scavenging activity was expressed as g
extracted by stirring with 25 mL of methanol at room equivalent quercetin per 100 g dry basis.
International Journal of Food Science and Technology 2014 © 2013 The Authors
International Journal of Food Science and Technology © 2013 Institute of Food Science and Technology
Desorption isotherms of two onion varieties A. A. Bouba et al. 447
© 2013 The Authors International Journal of Food Science and Technology 2014
International Journal of Food Science and Technology © 2013 Institute of Food Science and Technology
448 Desorption isotherms of two onion varieties A. A. Bouba et al.
absorb water (Magda et al., 2006). In this view, the Galmi Violet showed a higher desorption energy level
entire onion bulb of Galmi Violet variety exhibited compared with that of the Goudami. At intermediary
higher ability for water absorption compared with moisture, Goudami variety seemed to exhibit higher
Goudami. Monolayer moisture contents are very sorption energy, while no significant difference was
important in food technology because they define observed between both varieties at moisture higher
moisture contents suitable for food storage without than 39%. Such variations highlighted the difference
risk of deterioration. In this work, M0 values for the in the association of water molecules to structural
two varieties of onions at all temperatures corre- components in the bulb structure. At higher moisture
sponded to aw values <0.2. This has high technological content (>39%), water molecules were in the conden-
significance because when a commodity is stored at or sation region where they acted as free solvents. It was
below its critical moisture content, significant degrada- easily extracted from the bulb at low energy. In this
tion of quality can be prevented. EMC at water activ- condition, the extraction of water molecule did not
ity of 0.65 defines the critical moisture content below vary with the variety. At low moisture content, water
which food materials are stored without significant risk molecules were highly bound to the polar site of dry
of spoilage (Navarro and Donahaye, 2005 in Bup matter. More probably, the highly polar sites of Galmi
et al., 2013). Violet would attract more water molecules. This mois-
ture content interval was such that beyond 21% water
layers were free water and exhibited weak heat of
Heat of desorption
sorption. At the same time, the polar sites of the
The net isosteric heat of sorption can be used to Goudami variety would progressively attract water
estimate the energy required to allow water molecules molecules so as to increase the sorption heat more
to break away from the solid surface during dehydra- than that of Galmi Violet after 21%. The maximum net
tion. The moisture content at which the net isosteric isosteric heat was observed in the moisture content
heat of sorption approaches the latent heat of vapori- range from 0% to 14% with the Galmi Violet variety
sation of water is often taken as an indication of the exhibiting the highest value (32.58 kJ mol1), while the
amount of bound water existing in the food (Sharma Goudami variety had the lowest value (23.50 kJ mol1).
et al., 2009 in Ala’a et al., 2010). Sigma-plot (version 11.0 software) was used to fit
The values of the isosteric heat of sorption were cal- the experimental data of heats of sorption. Reverse
culated from the equilibrium moisture content at dif- third-order polynomial function gave a satisfactory
ferent temperatures with different moisture contents. prediction of heat of desorption (Qs) values as a func-
Figure S5 shows the variation in the net heats of the tion of water content (M) for the Goudami variety
sorption as a function of moisture content at 30 °C, (eqn 3) and Galmi Violet variety (eqn 4) data, each
45 °C and 60 °C and the corresponding prediction with a determination coefficient R2 = 0.99.
curves. The moisture content varied from 13% to
58.5% for the Goudami and from 14% to 56% for 764:29 16859:44 162159:97
Qs ¼ 9:37 þ þ ð3Þ
Galmi Violet varieties. It was observed that the curve M M2 M3
can be divided into three parts, namely moisture con-
1082:85 31347:54 347743:49
tent lower than 21% (however, an increase in the Qs ¼ 11:58 þ þ ð4Þ
moisture content was associated with a drastic M M2 M3
decrease in the net isosteric heat of desorption); mois-
ture content higher than 39% (with a little change in
Antioxidant activity
heat of desorption affecting the moisture content); and
moisture content between 21% and 39% (the interme- Tables S4 and S5 present the variation in total po-
diary part). Generally, the net isosteric heats of sorp- lyphenols and ferric and DPPH reducing effects of the
tion were high at low moisture contents, irrespective of slices of two onion varieties as influenced by water
the onion variety. Similar trends for many plant and activity and temperature. As expected, the total phe-
food materials have been reported in the literature: for nolic content significantly increased with increased
example, the works of Moreira et al. (2010) on chest- moisture content. In addition, the total phenols con-
nut and wheat flours from Spain, Bup et al. (2012) on tent decreased with increase in temperature from 30°C
shea nut (Vitellaria paradoxa Gaertn) from Cameroon, to 60°C. Change in total phenol content could be
Hamid (2010) on canola from Iran. This reflects the attributed to the enzymatic activity that could have
water binding strength and initial occupation of highly taking place in the bulb. According to Labuza (1984),
active polar sites to form a surface monolayer, fol- the enzymatic oxidation of polyphenols increased with
lowed by the progressive filling of the less available water activity. This concept seems to be validated in
sites (with lower bonding activation energies) (Ala’a this work with values ranging from 0.31 0.03 g (aw
et al., 2010). At moisture content lower than 21%, the 0.055) to 1.16 0.02 g gallic acid per 100 g d.b (aw
International Journal of Food Science and Technology 2014 © 2013 The Authors
International Journal of Food Science and Technology © 2013 Institute of Food Science and Technology
Desorption isotherms of two onion varieties A. A. Bouba et al. 449
0.836) for Galmi Violet variety and from 0.28 0.03 g the phenol content and the FRAP (r2 = 0.96; P < 0.05
(aw 0.055) to 1.51 0.06 g gallic acid per 100 g d.b for 30 °C, r2 = 0.92; P < 0.05 for 45 °C and 60 °C) or
(aw 0.836) for Goudami variety. It is important to DPPH reducing power (r2 = 0.98; P < 0.05 for 30 °C;
mention that onion bulbs are also consumed for their r2 = 0.97; P < 0.05 for 45 °C; r2 = 0.96; P < 0.05 for
antioxidant properties. Tables S4 and S5 show that 60 °C). The significant (P < 0.01) positive and linear
the remaining levels of TPC after drying at 45 °C and correlations observed between the phenol content
60 °C are 78.94% and 49.12%, respectively, for the and the antioxidant activities highlighted the role of
Goudami variety. Corresponding values for Galmi vio- phenols in the antioxidant activity of plant extracts.
let variety are 84%, 12% and 59.62%. With regard to The polyphenols present in fruits and vegetables like
the content of FRAP and DPPH, trends are similar to onions are potent antioxidants, and several authors
that of TPC. It is also observed from Tables S4 and have correlated the antioxidant activities of vegetables
S5 that FRAP still retains an after drying of 72.22% with their total phenol compound contents (Anna
and 50% and 52% and 36% at 45 and 60 °C, respec- et al., 2003; Amarowicz et al., 2004; Ramandeep &
tively, for Goudami and Galmi violet varieties. Con- Geoffrey, 2006; Santas et al., 2008; Abdou Bouba
cerning the DPPH, we note the activity of 33.33% for et al., 2010, 2012). In addition, numerous epidemio-
the same temperatures for the Goudami variety and logical and intervention studies suggested the correla-
37.78% and 25% at 45 and 60 °C, respectively, for tion between consumption of polyphenol-rich foods or
the variety Galmi Violet. This indicates that drying beverages and the prevention of certain stress-induced
had a negative impact on the antioxidant activity of chronic diseases such as cancers, neurodegenerative
two onion varieties. However, it has been demon- disorders, cardiovascular diseases and type 2 diabetes,
strated that tomato drying at 42 °C significantly or side effects of ageing (Arts & Hollman, 2005).
reduced its antioxidant contents (Toor and Savage, Furthermore, the positive and significant correlation
2006) and that shea nut (Vitellaria paradoxa Gaertn) coefficient was observed between the moisture content
from Cameroon drying at different temperatures and TPC (r2 = 0.959, P ≤ 0.05). Generally the FRAP
reduce considerably its tocopherol, which has an anti- oscillated from 0.09 0.02 g to 1.17 0.04 g ascor-
oxidant activity (Bup et al., 2011). The effect of tem- bic acid per 100 g d.b for Galmi Violet and from
perature was not important as that of aw on the 0.09 0.01 g to 1.01 0.03 g ascorbic acid per 100 g
phenol content, but it probably reflected the effect of d.b for Goudami. In addition, the DPPH reducing
temperature on the activity of enzymes involved in power was found between 0.02 g and 0.543 0.03 g
phenol oxidation. Generally, the high temperature quercetin per 100 g d.b for Galmi Violet and between
tends to destroy the enzymes and reduce their activity 0.01 g and 0.471 0.03 quercetin per 100 g d.b for
(Cheftel & Cheftel, 1977). In this respect, temperatures Goudami. DPPH reducing power and FRAP were sig-
of 45 °C and 60 °C seemed to be detrimental to oxi- nificantly low at high temperature and increased with
dative enzymes in onion bulbs. The negative effect of a decrease in temperature. In addition, the antioxidant
temperature on phenol content of onion slices was activities were significantly higher for Galmi Violet
reported in earlier studies (Akyıldız et al., 2004; Zano- onions and lower for Goudami variety. This difference
elo et al., 2006). Some authors reported an increase in in the activities of these varieties could be a reflection
phenol content with increased temperature as a result of their high levels of phenols as evident from its vio-
of the liberation of phenolic compounds from the let colour. Drying onions resulted in significant losses
matrix during the drying process. Comparatively, the in FRAP and DPPH reducing power for the two vari-
varieties exhibited different levels in phenols with sig- eties. A decline in total phenol content during dehy-
nificant interaction with temperature and water activ- dration was likely to be responsible for the observed
ity. There are many different values for the phenolic decrease in antioxidant activity (FRAP, DPPH reduc-
content of onion, which have been reported in previ- ing power) of dried onions. It should be noted, how-
ous studies. Bajaj et al. (1980) reported that the phe- ever that, the dried samples still contain significant
nol contents of onion samples varied between 1.85 amounts of antioxidant activity despite the negative
and 2.95 g per 100 g dry matter. Arslan & Ozcan effect of drying.
(2010) reported that the phenolic content ranged
between 0.472 and 1.66 g per 100 g dry matter. The
Conclusion
phenol contents of the dry onion in this study were
closer to these values, but were significantly higher Moisture sorption isotherms and the combined effect
than the values reported by Santas et al. (2008) in of temperature and water activity on the antioxidant
Spanish onion varieties. The total phenol contents activity of Goudami and Galmi Violet onion varieties
have always been associated with the antioxidant were studied. The EMC of the Galmi Violet onion
activity (Abdou Bouba et al., 2010, 2012). In this variety is significantly higher than that of the Goudami
study, we observed a significant correlation between variety, irrespective of the temperature and water
© 2013 The Authors International Journal of Food Science and Technology 2014
International Journal of Food Science and Technology © 2013 Institute of Food Science and Technology
450 Desorption isotherms of two onion varieties A. A. Bouba et al.
activity. Among the models tested, the GAB equation Ames, B.N., Shigenaga, M.K. & Hagen, T.M. (1993). Oxidants,
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© 2013 The Authors International Journal of Food Science and Technology 2014
International Journal of Food Science and Technology © 2013 Institute of Food Science and Technology
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Figure S1. Desorption of the isotherms of Goudami
Superheated steam drying of mate leaves and effect of drying onion variety at different temperatures.
conditions on the phenol content. Journal of Food Process Engi- Figure S2. Desorption of the isotherms of Galmi
neering, 29, 253–268. Violet onion variety at different temperatures.
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isotherms and moisture sorption hysteresis of intermediate
moisture content banana. Journal of Food Engineering, 86, ami and Galmi Violet onion varieties at 30 °C. (b)
342–348. Desorption of the isotherms of Goudami and Galmi
Violet onion varieties at 45 °C. (c) Desorption of the
isotherms of Goudami and Galmi Violet onion varieties
Supporting Information at 60 °C.
Additional Supporting Information may be found in Figure S4. Comparison of the experimental and pre-
the online version of this article: dicted desorption for the equilibrium moisture con-
Table S1. Water activity values of the saturated salt tents of the Goudami variety at 30 °C.
solutions at the used temperatures. Figure S5. Variation in the net isosteric heat for
Table S2. Equations used to describe the desorption Goudami and Galmi Violet onion varieties at 30 and
equilibrium isotherms. 60 °C.
Table S3. Estimated parameters and fitting criteria
of the models applied to the experimental desorption
data for Goudami and Galmi Violet onion varieties.
International Journal of Food Science and Technology 2014 © 2013 The Authors
International Journal of Food Science and Technology © 2013 Institute of Food Science and Technology