Innovative Food Science and Emerging Technologies 43 (2017) 45–53

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Innovative Food Science and Emerging Technologies

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Moisture sorption isotherms of high pressure treated fruit peels used as MARK
dietary fiber sources
Viridiana Tejada-Ortigoza, Luis Eduardo Garcia-Amezquita, Vinicio Serment-Moreno,
J. Antonio Torres⁎, Jorge Welti-Chanes⁎⁎
Tecnológico de Monterrey, Escuela de Ingeniería y Ciencias, Centro de Biotecnología FEMSA, Eugenio Garza Sada 2501, Monterrey, NL 64849, Mexico

A R T I C L E I N F O A B S T R A C T

Keywords: High hydrostatic pressure (HHP) treatments can improve the potential of orange, mango, and prickly pear peels
High hydrostatic pressure as food formulation fiber sources. Akaike Information Criteria differences identified Peleg and GAB as the best
Fruit peel dietary fiber model alternatives to describe experimental moisture isotherms. HHP (600 MPa/10 min/22 and 55 °C) effects on
Moisture sorption isotherm moisture isotherms expressed as relative water sorption content change with respect to controls (RWSCaw)
Moisture sorption hysteresis
showed that in the 0.1–0.93 aw range, HHP improved the adsorption water retention of orange peels. The same
Hygroscopic properties
was true for the desorption water retention for all HHP-treated fruit peels except for prickly pear HHP-treated at
Akaike Information Criteria
22 °C and > 0.35 aw. The area under the hysteresis curve (AH) in the 0.15–0.51 aw range showed that HHP
increased hysteresis for all fruit peels tested. All this illustrates the HHP potential to modify the hygroscopic
properties of fruit peels at lower temperature and in less processing time than conventional processes.
Industrial relevance: Orange, mango, and prickly pear peels are potential food fiber formulation sources with
differentiated hygroscopic and functional properties. In this study, 600 MPa treatments at 22 and 55 °C for
10 min modified the adsorption and desorption moisture retention capacity of all fruit peels tested in this study.
HHP technology can improve the potential of fruit peels as dietary fiber sources with the advantage of shorter
processing times and lower temperatures than conventional technologies used to treat food fibers.

1. Introduction
In Latin America alone, the food industry generates ~56 million
tons of waste from the production, processing, handling and storage of
fruits and vegetables (Santivañez, 2014). These worldwide-generated
waste materials, including peel, cores, pips, kernels, skins, and stems,
are potential sources of functional ingredients such as dietary fiber
(DF). By-products from apple, grape, lemon, mango, orange, and other
fruits have been used as non-conventional DF sources (O'Shea,
Arendt, & Gallagher, 2012; O'Shea et al., 2015; Tejada-Ortigoza, Garcia-
Amezquita, Serna-Saldívar, & Welti-Chanes, 2015). However, thermal
(Benítez et al., 2011), chemical (Šoronja-Simović et al., 2016), enzy-
matic (Laurikainen, Härkönen, Autio, & Poutanen, 1998), and other
processes (Chau, Wang, & Wen, 2007; Chen, Gao, Yang, & Gao, 2013;
Zhu, Du, Li, & Li, 2014) are required to extract DFs, modify their
technological functionality and convert these residues into food in-
gredients with desirable properties. These treatments modify their
properties including their total (TDF), soluble (SDF) and insoluble (IDF)
dietary fiber content.
Treating onion bagasse at 115 °C for 31 min increased the SDF
content from 8.8 to 10.5% (db) while the relationship SDF/TDF in-
creased from 24.4 to 30.6% (Benítez et al., 2011). Chemical modifica-
tion of sugar beet fibers dried at 55 °C using H2O2 (30% v/v), NaOH
(10 M) and HCl (35% v/v) for ~24 h increased the SDF content and the
DF/TDF from 13.9 and 18.7% (db) for untreated to 17.6 to 23.9% (db)
for treated samples, respectively (Šoronja-Simović et al., 2016). As
previously reviewed (Tejada-Ortigoza et al., 2015), chemical mod-
ification methods involve the use of large amount of solvents, long
processing time (0.5–30 h), and high temperature (60–100 °C). This has
raised an interest in non-thermal technologies, including high hydro-
static pressure (HHP), as an alternative for DF modifications. For ex-
ample, Tejada-Ortigoza, Garcia-Amezquita, Serna-Saldívar, & Welti-
Chanes, (2017) showed that the DF content is affected by HHP treat-
ments and that the modifications observed varied with the food matrix.
Treating mango and orange peel samples for 10 min at 600 MPa and
55 °C increased the SDF content from 15.2 to 17.5% (db) and from 3.7
to 5.9% (db), respectively. In addition, the SDF/TDF ratio increased
from 37.4 and 7.3% (db) for untreated mango and orange peels to 42.2

⁎
Corresponding author at: Tecnológico de Monterrey, Escuela de Ingeniería y Ciencias, PO Box 2015, Corvallis, OR 97339, USA.
⁎⁎
Corresponding author at: Tecnológico de Monterrey, Escuela de Ingeniería y Ciencias, Eugenio Garza Sada 2501, Col. Tecnológico, Monterrey, NL, Mexico.
E-mail addresses: dr.j.antonio.torres@gmail.com (J.A. Torres), jwelti@itesm.mx (J. Welti-Chanes).

http://dx.doi.org/10.1016/j.ifset.2017.07.023
Received 15 March 2017; Received in revised form 6 July 2017; Accepted 8 July 2017
Available online 15 July 2017
1466-8564/ © 2017 Elsevier Ltd. All rights reserved.
V. Tejada-Ortigoza et al.
and 10.8% (db), and to 45.0 and 12.0% (db), when treated at 600 MPa
at 22 and 55 °C, respectively. On the other hand, 10 min treatments at
600 MPa of prickly pear peel increased the IDF content from 32.6% (db)
for untreated samples to 35.5 and 38.1% (db) for HHP treatments at 22
and 55 °C, respectively. In the case of prickly pear peel, TDF content
increased up to 4.8 and 5.7% (db) after HHP treatments at 22 and 55 °C,
respectively (Tejada-Ortigoza et al., 2017). Treatments at 200 and
400 MPa at 60 °C for 15 min increased okara's SDF content about 2.8
and 8.1 times, respectively (Mateos-Aparicio, Mateos-
Peinado, & Rupérez, 2010). Under these conditions, the SDF/TDF ratio
increased from 4.6% (db) for untreated okara to 11.1 and 37.2% (db),
respectively. When aided by 0.025% of the food grade enzyme Ul-
traflo®, 30 min treatments at 600 MPa and 40 °C increased the okara
total soluble carbohydrate content from 9 to 15.6% (db) (Pérez-López,
Mateos-Aparicio, & Rupérez, 2016). Conversely, a 500 MPa treatment
at 20 °C reduced the SDF content of untreated white cabbage from 7.6
to 5.9% (db) (Wennberg & Nyman, 2004).
The review of previous work shows that HHP treatments can change
the content and properties of fruit peels DF and could widen their range of
technological applications. Sorption isotherms are a potentially useful tool
to analyze fruit peel modifications induced by HHP treatments since hy-
groscopic properties of food materials depend on their SDF and IDF con-
tent and SDF/TDF ratio. The relationship between equilibrium moisture
content (EMC) and water activity (aw) at constant temperature and under
equilibrium conditions is graphically expressed as moisture isotherm
curves. Moisture sorption phenomena are not fully reversible and the EMC
difference between adsorption and desorption values is known as hyster-
esis Al-Muhtaseb, McMinn, & Magee, 2004. Mathematical models used to
describe and analyze water sorption properties of foods include those
based on theoretical concepts such as the monolayer moisture value (BET,
GAB), or they are semi-empirical (Iglesias and Chirife), and empirical
expressions (Oswin, Kühn, Peleg). Standard statistical criteria such as R2
are not always able to determine the best model to describe experimental
data. In such cases, statistic tools such as the Akaike Information Criteria
(AIC) can be used to evaluate the goodness of fit while penalizing the use
of an excessive number of parameters. AIC determines, among a set of
models, which one is the best to use by supplying information on the
strength of the evidence for each model and considering the information
lost when the model is used to approximate experimental data
(Posada & Buckley, 2004; Serment-Moreno, Fuentes, Barbosa-Cánovas,
Torres, & Welti-Chanes, 2015).
A few studies have reported the effect of HHP treatments on the
hygroscopic properties of treated materials. Increasing the pressure
holding time at 20 °C of 300 MPa treatments of maize starch suspen-
sions have been shown to shift isotherm curves to higher EMC values
and increase the hysteresis effect at aw > 0.44 (Santos et al., 2014).
Conversely, 15 min treatments at 300 and 500 MPa of a starch solution
at 20 °C showed that increasing the pressure level decreased the hys-
teresis effect (Santos et al., 2014). In the case of brown rice, 300 MPa
treatments had lower EMC values than samples treated at higher
pressure (400, 500 MPa) (Yu et al., 2015). The authors stated that HHP
treatments might have cracked the brown rice kernels resulting in the
higher EMC value observed at higher pressure. In addition to HHP
treatment effects, changes induced by homogenization, osmotic dehy-
dration and convection drying in the EMC and GAB parameters of food
materials have been evaluated too. Homogenization (8000 rpm, 3 min)
affected the tissue structure of freeze dried strawberry reducing its EMC
by 5 g water/100 g ds at aw ~ 0.6 (Moraga, & Martı́nez-Navarrete,
N.,, & Chiralt, A., 2004). Osmotic dehydration in 25 g/L calcium lactate
solution and convection drying (70 °C/10 g/kg dry air, 0.5 m/s) treat-
ments lowered papaya M0 values from 37.5 to 13.1 and 11.5 g water/
100 g ds, respectively. These reductions were attributed to changes in
sugar content due to the osmotic dehydration and structural mod-
ifications caused by convection drying (Udomkun, Argyropoulos,
Nagle, Mahayothee, & Müller, 2015). In general, structure and compo-
sition changes are responsible for the modifications of the moisture
46
Innovative Food Science and Emerging Technologies 43 (2017) 45–53
sorption capability of DF sources. Changes in the hygroscopic properties
of HHP-treated fruit peels would allow explain their functionality as
food ingredients and their role in digestive processes and other health
benefits of DFs (Gurak, De Bona, Tessaro, & Marczak, 2014). The ana-
lysis of hygroscopic properties based on sorption isotherms is needed to
evaluate modifications of the water adsorption or desorption capacity
of fruit peels treated by HHP. Therefore, this study focuses on evalu-
ating the effect of HHP treatments at room and moderate temperature
on the moisture isotherms of mango, orange, and prickly pear peels.
2. Material and methods
2.1. Fruit peel samples
Mango (Mangifera indica L. cv Ataulfo), orange (Citrus sinensis L.)
and prickly pear (Opuntia ficus-indica cv Verde Villanueva) purchased at
a local supermarket (Monterrey, N.L., Mexico) were immersed 10 min
in chlorinated water (15 ppm). Fruit peel was then manually removed,
ground (VM0103, Vitamix, Cleveland, OH), vacuum packed (model
EVD 4; Torrey, Monterrey, N.L., Mexico) in 12 × 15 cm polyethylene
bags (Filmpack SA de CV, Guadalupe, N.L., Mexico) and stored at 4 °C
until use within 2 h.
2.2. High hydrostatic pressure (HHP) processing of fruit peel
Polyethylene pouches (~ 11 × 7 × 1 cm) with ~50 g peel samples
were treated in duplicate runs at 600 MPa for 10 min (2 L Welch food
processor, Avure Technologies, Middletown, OH) using water at 22 or
55 °C as the pressurizing fluid and reaching during pressure holding an
average temperature of 30.5 ± 1.4 and 65.9 ± 2.5 °C, respectively. A
430 MPa min− 1 compression rate yielded a 1.4 min come-up time
(CUT) to 600 MPa while decompression was almost instantaneous
(< 5 s). Samples were stored at − 80 °C immediately after processing
and used within 8 weeks.
2.3. Moisture sorption isotherms
Untreated (control) and HHP-treated peel samples were freeze-dried
at − 50 °C and 2.0 mbar (Labconco, Kansas City, MO), hand-milled,
sieved through a mesh number 40 (425 μm), and stored in desiccators
containing P2O5 (25 °C) at least for 5 days before analysis. Initial
moisture content was determined as specified by AOAC Official Method
920.151. Duplicate adsorption and desorption moisture isotherms in
the ~0.10 to 0.93 aw range were determined at 30 °C with ± 0.0001
aw resolution following the device manufacturer's instructions
(Aquasorp Isotherm Generator, Decagon Devices Inc., Pullman, WA).
2.4. Isotherm modelling
The GAB, Iglesias and Chirife, Oswin, Kühn and Peleg models (Eqs.
1–5, Table 1) previously reported for similar materials were used to
describe moisture sorption isotherm data (Caballero-Cerón, Guerrero-
Beltrán, Mújica-Paz, Torres, & Welti-Chanes, 2015). Parameters for
each model were estimated using the least-square method and the Mi-
crosoft Excel solver function. Model fit was evaluated based on values
for the coefficient of determination (R2, Eq. (6)) and residual sums of
squares (SSE, Eq. (7)), where yi and yi are the moisture experimental
observation and estimated value, respectively.
∑ (yi − 
yi )2
R2 = 1 −
∑ (yi − yi )2 (6)
SSE = ∑ (yi − yi )2 (7)
Model selection was performed with the AIC (Eq. (8)), which eval-
uates the goodness of fit (first term) and penalizes the excessive use of
V. Tejada-Ortigoza et al. Innovative Food Science and Emerging Technologies 43 (2017) 45–53

Table 1 HHP effect on the hygroscopic properties of fruit peels. The relative
Mathematic models used to describe moisture sorption isothermsa. water sorption change (RWSCaw) induced by HHP was expressed as
follows (Eq. (13)):
Model Equation
Mt − Mc
GAB M0 CKaw (1) RWSCaw =
M= Mc (13)
(1 − Kaw )(1 − Kaw + CKaw )
Iglesias and Chirife A + BT
1 (2) where Mc and Mt. are the EMC values of control and HHP-treated
−e C
M=⎡ ⎤
⎢
⎣ ln(aw ) ⎥
⎦
samples, respectively, evaluated at the same aw.
Oswin aw ⎤
B (3)
M = A⎡
⎢
⎣ 1 − aw ⎥
⎦ 3. Results and discussion
Khün A (4)
M= 1
+B
ln
aw
3.1. Sorption isotherms of mango, orange and prickly pear peel
Peleg M = k1awn1 + k2awn2 (5)
Mango, orange, and prickly pear peel moisture isotherms showed
a
M and M0 are the equilibrium and monolayer moisture content (g water/100 g ds ), the same typical BET type III behavior but differed in water adsorption
respectively; C and K are dimensionless parameters related to heat of sorption in the
and desorption capacity (Fig. 1). As reported for orange peel and
monolayer and multilayer region respectively; k1, k2, n1 and n2 are dimensionless para-
meters; A, B and C are constants prickly pear seeds, type III behavior occurs when sugars and other so-
luble crystalline components are present and thus the sharp moisture
model parameters (second term), where σ 2̂ is the maximum likelihood isotherm increase at aw > 0.70 reflects sugar dissolution in the sorbed
estimator of the variance and p is the number of model parameters. AIC water vapor (Edrisi Sormoli & Langrish, 2015; Hassini, Bettaieb,
varies among datasets and thus differences with respect to the model Desmorieux, Torres, & Touil, 2015; Kammoun Bejar, Boudhrioua
with the minimum AIC are used instead (Δ AIC; Eq. (9)) to indicate Mihoubi, & Kechaou, 2012; Rahman, 1995; Santos et al., 2014). Ad-
strong (Δ AIC ≤ 2), moderate (2 < Δ AIC ≤ 4) or slight (Δ AIC > 4) sorption and desorption isotherms showed that prickly pear peel dis-
model support evidence (Burnham & Anderson, 2002). played higher EMC values, followed by mango and orange. Even though
the SDF content of prickly pear peel is not the largest among the tested
n
AIC = − ln σ 2̂ + 2p fruit peels (Tejada-Ortigoza et al., 2017), its moisture sorption prop-
2 (8)
erties reflect its SDF and IDF polysaccharide composition. Prickly pear
∆AICi = AICi − AICmin (9) peel is mainly composed of mucilage, pectin, cellulose and hemi-
cellulose, i.e., polysaccharide chains with polar functional groups such
as carboxyl, hydroxyl, sulfate, phosphate, aldehydes, and ketones with
2.5. Sorption surface area
extensive water binding (Barka, Ouzaouit, Abdennouri, & Makhfouk,
2013; Habibi, Mahrouz, & Vignon, 2009; Lira-Ortiz et al., 2014). Re-
The sorption surface area (Eq. (10)) of a material is closely related
flecting its composition and moisture sorption characteristics, prickly
to its monolayer moisture value (M0) and is estimated as follows (K.
pear peel has been used as emulsifier, thickener, plasticizer, and more
Moraes & Pinto, 2012; Yogendrarajah, Samapundo, Devlieghere, De
recently as a moisture biosorbent (Barka et al., 2013).
Saeger, & De Meulenaer, 2015):
1 3.2. Isotherm model fit
S0 = M0 N0 A H2 O = 35.3 M0
MWH2 O (10)
GAB, Iglesias and Chirife, Oswin, Kühn and Peleg models have been
where S0 is the sorption surface area (m2/g solids), M0 was calculated
previously reported to describe isotherms for materials similar to the
using the GAB model, N0 is the Avogadro number (6.0 × 1023 mole-
fruit peels included in this study (Caballero-Cerón et al., 2015; Edrisi
cules/mol), AH2O is the area of a water molecule (1.06 × 10− 19 m2),
Sormoli & Langrish, 2015). Model selection using only R2 is difficult
and MWH2O is the molecular weight of water (18 g/mol). The parameter
when all alternatives fit the data well, as in the case of the models
S0 was also used as criteria to evaluate changes caused by HHP treat-
evaluated in this study using adsorption (R2 > 0.97, Table 2) and
ments in the sorption properties of fruit peels.
desorption (R2 > 0.99, Table 3) EMC isotherm data. In the present
study, AIC was used for model selection providing statistical evidence
2.6. Sorption hysteresis phenomena to choose the best options as reported by Serment-Moreno et al. (2015).
AIC showed that the Peleg model was the best alternative to describe
Hysteresis (Haw, Eq. (11)) was determined as the difference between adsorption (ΔAICi ≤ 2 except for orange peel treated at 600 MPa and
desorption (Mdes) and adsorption (Mads) EMC values predicted with the 55 °C, Table 2) and desorption data (ΔAICi = 0, Table 3).
Peleg model (Eq. (5)) as a function of aw for each fruit peel:
Hysteresis = Haw = Mdes − Mads (11) 3.2.1. Effect of high hydrostatic pressure on sorption isotherms model
parameters
As a global criterion for quantifying changes in the hysteresis phe-
Although GAB was ranked second best alternative according to AIC,
nomenon, the area of hysteresis (AH) was defined as the integral of the
this model yielded R2 ≥ 0.985 for all isotherms and its parameters
Haw change as a function of the change in aw. AH was calculated and
allow a physical interpretation of moisture sorption isotherm data
quantified by applying the trapezoidal rule to increments of 0.02 aw
(Basu, Shivhare, & Mujumdar, 2006). Estimated values of parameter K
units, at defined intervals of aw (Eq. (12)).
(related to the multilayer heat sorption) ranged from 0.940 to 0.989 for
AH = ∫ Haw daw (12)
mango, orange, and prickly pear peel, and were not affected by the
pressure-temperature conditions tested in this study (Table 4). Con-
versely, parameter C (related to the monolayer heat sorption) increased
2.7. Relative water sorption changes of mango, orange and prickly pear peel for orange adsorption and all desorption moisture isotherms of HHP-
induced by HHP treated fruit peels. In the case of orange and prickly pear peel HHP-
treated at 55 °C, C parameter increased up to 5.4 and 1.9 times, re-
Changes in adsorption or desorption EMC values estimated as a spectively, when compared to untreated samples. Greater C values
function aw with the Peleg equation (Eq. (5)) were used to assess the suggest that water is more strongly attached to the food matrix and thus

47
V. Tejada-Ortigoza et al. Innovative Food Science and Emerging Technologies 43 (2017) 45–53

Fig. 1. A) Water adsorption and B) desorption isotherms of fruit

100 peels at 30 °C.
Mango A
90 Orange
Prickly pear
Moisture content (g H2O/ 100 g dry solids)

80

70

60

50

40

30

20

10

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
aw

100
Mango B
90 Orange
Prickly pear
Moisture content (g H2O/ 100 g dry solids)

80

70

60

50

40

30

20

10

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
aw

more energy is required for its removal (Edrisi Sormoli & Langrish,
2015; Velázquez-Gutiérrez et al., 2015).
HHP treatments increased M0 values for orange (adsorption), mango
(adsorption and desorption) and prickly pear (adsorption). In the case
of orange desorption isotherms, M0 was reduced from 13.27 g water/
100 g ds for untreated sample to 8.12 and 7.54 g water/100 g ds for
HHP samples treated at 22 and 55 °C, respectively, while those for
prickly pear were reduced from 15.1 (untreated sample) to 11.7 and
11.6 g water/100 g ds. The decrease in M0 values observed in this study
may reflect a reduction in the available water binding sites caused by
physicochemical and structural changes, occurring mainly at low aw
values where the monolayer concept is of practical relevance
(Velázquez-Gutiérrez et al., 2015). Sorption isotherms for orange peel
at 30 °C have been previously reported by Edrisi Sormoli & Langrish,
(2015). Their reported M0 value at 30 °C, 8.7 g water/100 g ds is
comparable to the 7.13 g water/100 g ds value obtained in this study
for the same matrix. Similarly, at this temperature, the M0 reported for
lemon peel was 6.9 g water/100 g ds (García-Pérez, Cárcel,
Clemente, & Mulet, 2008).
S0 reflects the number and size of pores and plays an important role
in the analysis of the water binding properties of foods. Due to their
proportionality, S0 behaves similarly to M0. Both, S0 and M0, change
with the total number of active sites for water binding induced by
processing modifications (Velázquez-Gutiérrez et al., 2015). HHP
treatments increased S0 values in orange, mango, and prickly pear peels
adsorption isotherms (Table 5) indicating a larger availability of active
moisture binding sites. Mango, orange and prickly pear values for ad-
sorption and desorption isotherms were 308.5–418.7, 251.8–468.4 and
304.2–531.5 m2/g. These values are higher than the S0 values at 30 °C
for texturized soy protein and whole black peppercorn, 192.2 and
125.6 m2/g, respectively (Cassini, Marczak, & Noreña, 2006;
Yogendrarajah et al., 2015). Labuza, (1968) also reported values in the
100–250 m2/g range for several food materials. However, the high
values reported in this study are typical of materials with a microporous
structure (Velázquez-Gutiérrez et al., 2015). The S0 value at 25 °C re-
ported for freeze-dried chia mucilage is 277.5 m2/g and similar to those
determined at 20 °C for dried and texturized potato slices, 243.5 and
374.2 m2/g respectively (Iguedjtal, Louka, & Allaf, 2008; Velázquez-

48
V. Tejada-Ortigoza et al. Innovative Food Science and Emerging Technologies 43 (2017) 45–53

Table 2
Statistical summary of model fit to adsorption isotherm curves of fruit peels.

Model Statistical criteria Mango Orange Prickly pear

Untreated 22 °C 55 °C Untreated 22 °C 55 °C Untreated 22 °C 55 °C

GAB R2 0.996 0.996 0.995 0.999 0.998 0.999 0.990 0.998 0.995
SSE 169.7 184.5 249.3 57.9 68.5 54.5 1208.2 207.5 603.4
AIC − 0.4 24.4 76.4 − 204.6 − 168.0 −213.5 347.8 29.8 224.5
ΔAICi 128.3 238.6 341.4 209.0 155.8 0.0a 4.9 41.6 38.6
Iglesias & Chirife R2 0.988 0.984 0.980 0.992 0.991 0.992 0.988 0.992 0.988
SSE 537.8 840.1 1040.7 438.9 475.4 360.0 1491.6 836.7 1519.8
AIC 183.8 272.5 304.5 164.1 178.8 128.1 383.5 281.6 392.5
ΔAICi 312.6 486.7 569.5 577.7 502.6 341.6 40.7 293.4 206.6
Oswin R2 0.996 0.993 0.990 0.998 0.997 0.998 0.990 0.997 0.993
SSE 194.3 387.7 544.7 128.5 134.0 82.3 1188.5 320.8 816.5
AIC 21.4 144.9 200.2 − 60.7 − 49.2 −140.5 342.9 107.2 278.2
ΔAICi 150.1 359.1 465.3 352.9 274.6 72.9 0.0a 118.9 92.3
Khün R2 0.979 0.977 0.976 0.990 0.982 0.981 0.988 0.992 0.988
SSE 834.0 1036.9 1094.7 445.0 788.4 721.1 1446.9 714.4 1292.3
AIC 277.8 307.3 312.6 166.6 269.9 254.6 378.1 252.9 362.7
ΔAICi 406.6 521.5 577.6 580.2 593.7 468.0 35.2 264.6 176.8
Peleg R2 0.998 0.999 0.999 0.9996 0.999 0.998 0.990 0.998 0.996
SSE 80.9 42.9 29.5 18.3 28.5 68.4 1171.1 163.3 483.8
AIC − 128.8 − 214.2 − 265.0 − 413.6 − 323.8 −170.1 344.2 − 11.7 185.9
ΔAICi 0.0a 0.0a 0.0a 0.0a 0.0a 43.4 1.4a 0.0a 0.0a

a
Substantial evidence supporting model fit (ΔAIC ≤ 2)

Gutiérrez et al., 2015). Even higher values, 588.0 and 374.5 m2/g at 50
and 70 °C, respectively, have been reported for apple (M. A. Moraes,
Rosa, & Pinto, 2008).
3.2.2. Sorption hysteresis
Sorption hysteresis is related to the differences in the energy needed
to fill or empty the capillaries and binding sites of a food material (Al-
Muhtaseb et al., 2004). In the low aw range, all HHP-treated fruit peels
presented higher Haw values than untreated samples (Fig. 2). At high aw
values, this was also true for all fruit peels except for that form mango
which decreased for aw > 0.35 when treated at 22 °C, and showed no
practical differences for aw > 0.60 when treated at 55 °C. In the case of
orange peel at aw ≤ 0.5, Haw values for untreated samples reached
0.65 g/100 g ds compared to 2.5 and 2.1 g/100 g ds for samples HHP-
treated at 22 and 55 °C, respectively. In the same aw range, untreated
mango and prickly pear reached Haw values of 3.2 and 2.4 g/100 g ds
while samples HHP-treated at 22 °C yielded values of 5.1 and 3.9 g/
100 g ds, respectively, and those HHP-treated at 55 °C yielded values of
4.9 and 5.4 g/100 g ds, respectively. In the case of orange and prickly
pear fruit peels negative Haw values were observed in the at ~0.51 to
~0.71 aw, range. These negative values reflect an interesting behavior,
i.e., desorption moisture values fell below those for adsorption.
The hysteresis phenomena were also evaluated by estimating the
area under the Haw curve (AH) in two aw regions, 0.15 to 0.51 and 0.71
to 0.93. The highest AH values were determined for mango peel fol-
lowed by prickly pear and orange peel. In the 0.15 to 0.51 aw range,
HHP treatments yielded higher AH values, i.e., higher capacity to retain
water. In the case of orange peel, HHP treatment increased AH from

Table 3
Statistical summary of model fit to desorption isotherm curves of fruit peels.

Model Statistical criteria Mango Orange Prickly pear

Untreated 22 °C 55 °C Untreated 22 °C 55 °C Untreated 22 °C 55 °C

2
GAB R 0.991 0.995 0.997 0.9995 0.998 0.997 0.985 0.997 0.995
SSE 491.8 359.9 163.9 22.4 121.3 142.2 1947.1 367.5 732.9
AIC 186.2 133.5 5.9 −302.4 − 60.8 − 32.8 402.8 135.3 256.2
ΔAICi 57.1 122.0 171.2 114.8 106.3 105.0 11.6 144.6 139.3
Iglesias and Chirife R2 0.984 0.988 0.992 0.987 0.991 0.993 0.976 0.991 0.990
SSE 906.3 823.0 540.3 711.6 541.0 429.0 3110.3 1096.8 1344.2
AIC 285.1 272.1 199.5 241.8 201.7 160.7 474.8 326.8 359.7
ΔAICi 156.0 260.6 364.8 659.0 368.9 298.5 83.6 336.1 242.8
Oswin R2 0.988 0.992 0.995 0.994 0.996 0.996 0.981 0.995 0.993
SSE 644.9 516.8 282.3 331.5 241.6 210.5 2457.6 640.1 949.7
AIC 228.9 193.0 93.1 121.1 59.1 34.7 437.6 231.5 299.3
ΔAICi 99.8 181.5 258.3 538.3 226.2 172.4 46.4 240.8 182.4
Khün R2 0.971 0.972 0.980 0.983 0.979 0.981 0.972 0.987 0.985
SSE 1566.9 1806.3 1240.7 786.2 1122.0 998.3 3529.4 1476.2 1901.9
AIC 375.4 405.8 335.9 257.5 330.9 310.2 494.8 379.4 420.1
ΔAICi 246.3 394.2 501.1 674.7 498.0 448.0 103.6 388.7 303.2
Peleg R2 0.994 0.997 0.999 0.9998 0.999 0.999 0.986 0.999 0.997
SSE 343.7 173.6 57.0 10.7 65.8 77.7 1786.5 160.6 325.4
AIC 129.1 11.5 − 165.2 −417.2 − 167.2 − 137.8 391.2 − 9.3 116.9
ΔAICi 0.0a 0.0a 0.0a 0.0a 0.0a 0.0a 0.0a 0.0a 0.0a

a
Substantial evidence supporting model fit (ΔAIC ≤ 2)

49
V. Tejada-Ortigoza et al. Innovative Food Science and Emerging Technologies 43 (2017) 45–53

Table 4
Estimated GAB and Peleg sorption model parameters for fruit peels.

Model Parameter Mango Orange Prickly pear

Untreated 22 °C 55 °C Untreated 22 °C 55 °C Untreated 22 °C 55 °C

Adsorption
GAB M0 10.12 10.05 11.86 7.13 7.36 7.35 8.62 9.61 11.33
C 0.90 0.84 0.59 1.01 1.40 1.89 1.60 0.92 0.78
K 0.92 0.94 0.93 0.96 0.96 0.96 0.99 0.97 0.96
Peleg k1 36.5 49.4 53.3 35.0 36.2 31.6 50.5 53.0 61.1
k2 92.7 128.1 141.5 104.4 99.1 87.8 212.0 170.0 185.2
n1 2.08 2.63 2.90 2.35 2.13 1.75 2.23 2.61 2.76
n2 14.57 20.05 22.32 15.80 15.69 12.77 17.71 17.85 18.73

Desorption
GAB M0 8.74 9.25 8.79 13.27 8.12 7.54 15.06 11.67 11.62
C 1.76 2.28 2.10 0.44 1.68 2.38 0.70 0.98 1.35
K 0.94 0.95 0.95 0.92 0.95 0.96 0.94 0.95 0.96
Peleg k1 14.2 14.8 17.1 23.12 17.2 17.3 24.4 18.0 18.1
k2 82.1 88.2 89.3 81.10 81.9 82.5 133.4 127.8 136.3
n1 0.72 0.62 0.80 1.77 0.99 0.91 1.19 0.89 0.73
n2 6.60 6.34 7.07 8.79 7.56 7.65 7.98 7.67 7.39

Table 5
Specific surface area of sorption of fruit peels (m2/g).
Peel Adsorption Desorption
Control 600 MPa/ 600 MPa/ Control 600 MPa/
22 °C 55 °C 22 °C
Mango 357.3 354.7 418.7 308.5 326.6
Orange 251.8 260.0 259.3 468.4 286.6
Prickly pear 304.2 339.3 399.9 531.5 411.8
0.174 (untreated) to 0.721 and 0.532 when HHP-treated at 22 and
55 °C, respectively. In the same aw range, HHP-treatment of mango peel
increased AH values from 0.893 to 1.567 and 1.580 when pressurized at
22 and 55 °C, respectively. In the case of prickly pear, HHP treatments
at 22 and 55 °C yielded AH values of 1.164 and 1.653, i.e., again higher
than the 0.662 value for untreated samples. In the 0.71 to 0.93 aw
range, smaller and less consistent differences between HHP-treated and
control samples were observed with AH values in the 0.547–0.740,
0.847–1.104 and 1.087–1.253 range for orange, mango, and prickly
pear peel, respectively. For intermediate aw values, negative AH values
were determined for orange and prickly pear peel, i.e., Mads > Mdes. All
these findings are related to the fruit fiber composition and the re-
arrangements of structure and conformation caused by HHP treatments
which altered the moisture binding of sorption sites. A relation can be
found between the SDF content of the peel fruit Tejada-Ortigoza et al.,
2017 and the AH values here determined. The higher the SDF content,
the higher the AH (mango > prickly pear > orange). Yu et al. (2015)
also reported an hysteresis increase reaching 5.3%, in brown rice after a
300 MPa treatment for 10 min.
3.2.3. Relative water sorption changes of mango, orange and prickly pear
peel induced by HHP
Changes induced by HHP on the moisture sorption capacity of fruit
peels differed between adsorption (Fig. 3A) and desorption (Fig. 3B)
moisture content values. At aw < 0.64, sorption RWSCaw values
(Fig. 3A) for mango peel samples HHP-treated at 55 and 22 °C reached
negative RWSCaw values of − 0.58 and −0.75, respectively, while both
samples reached ~ 0.10 at aw = 0.75. In the case of prickly pear, HHP
treatments resulted in negative RWSCaw values over all the studied aw
range, with exception of the sample treated at 55 °C in the 0.70 to 0.88
aw range, where a slight increase in the adsorption EMC resulted in
RWSCaw values of ~0.03. When HHP-treated at 55 °C, prickly pear peel
adsorption isotherms reached negative RWSCaw values of − 0.64 at
aw = 0.10, the lowest aw included in this study. Negative RWSCaw
values indicate that some HHP treatments reduced the moisture ad-
sorption capacity of the fruit peel.
In the aw range studied, the desorption RWSCaw values (Fig. 3B) for
mango peel HHP-treated at 22 °C ranged 0.08–0.30 with a maximum at
600 MPa/ the lowest aw value studied (0.11). EMC modifications induced by HHP
55 °C reflect previously reported changes in DF profile and the SDF/TDF ratio
(Tejada-Ortigoza et al., 2017). After 600 MPa treatments at 22 and
310.4
55 °C for 10 min, the SDF content of mango peel was 17.0 and 17.5%
266.0
410.2 (db), respectively. Among the fruit peels studied a higher initial SDF
content was reported for mango (Tejada-Ortigoza et al., 2017); how-
ever, the DF profile modification induced by HHP treatment resulted in
lower RWSCaw values for mango than for orange peel. In the case of
orange peel, the largest RWSCaw values for adsorption and desorption
were achieved at aw ≤ 0.15, reaching 3.9 and 7.5, and 0.8 and 5.9
when treatments were performed at 55 and 22 °C, respectively. Despites
the orange's peel low SDF content, 3.7% (db), the increase induced by
HHP treatment at 22 and 55 °C, 5.4 and 5.9% (db) respectively, led to
materials with different hygroscopic properties. An increase in the SDF/
TDF, 7.3% for the untreated sample and 12.0% for the 55 °C HHP-
treated sample, was also observed (Tejada-Ortigoza et al., 2017). After
applying a HHP treatment at 55 °C, prickly pear peel desorption
reached RWSCaw values of 1.1 at aw = 0.10. The negative RWSCaw
values may reflect the increased IDF content, from 32.6% (db) for un-
treated to 38.1% (db) for the 600 MPa/55 °C/10 min treated sample,
only displayed for this fruit peel.
4. Conclusions
Orange, mango, and prickly pear peels are potential fiber sources
with different hygroscopic and functional properties. This study showed
that HHP treatments of these fiber sources can modify them. HHP ef-
fects on the adsorption and desorption moisture isotherms were de-
scribed by a new and useful parameter, relative water sorption change
(RWSCaw). Changes in RWSCaw values, and the hysteresis increases in-
duced by HHP treatments, and quantified in this study by a new and
useful parameter (AH), reinforce the possibility of using HHP as a novel
approach to produce fruit fibers with greater capacity to retain water
and improved food formulation applications. HHP allowed these
modifications using shorter processing times and at lower temperatures
than conventional technologies used to treat food fibers.
Among untreated fruit peels, prickly pear peel displayed larger
water sorption capacity, followed by mango and orange. In addition to
standard statistical criteria such as R2, Δ AIC values were used to select
Peleg and GAB as the two best alternatives to select a model to describe

50
V. Tejada-Ortigoza et al. Innovative Food Science and Emerging Technologies 43 (2017) 45–53

Fig. 2. Effect of 600 MPa and 10 min treatment on the hysteresis

phenomena of A) mango, B) orange and C) prickly pear modelled

9.0
Untreated
22 °C
A with Peleg equation as a function of aw.
55 °C

7.0
Hysteresis (g/ 100 g dry solids)

5.0

3.0

1.0

0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

-1.0
aw

Untreated
22 °C
B
9.0
55 °C

7.0
Hysteresis (g/ 100 g dry solids)

5.0

3.0

1.0

0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

-1.0
aw

Untreated
9.0 22 °C C
55 °C

7.0
Hysteresis (g/ 100 g dry solids)

5.0

3.0

1.0

0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

-1.0
aw

the moisture isotherms for the products studied. The Peleg model was
used to estimate changes in moisture sorption capacity and hysteresis of
HHP-treated fruit fibers, while the GAB parameters were used for a
physical interpretation of the changes in adsorption and desorption
isotherms. HHP treatment modified the GAB model parameters C, M0
and the related S0 value but not the parameter K.
Structural and compositional changes in fruit peels due to HHP
treatments could be related to modifications of the values reported in
this study. For example, previously reported modifications (Tejada-
Ortigoza et al., 2017) in the DF composition and SDF/TDF ratio caused
by HHP treatments at 22 and 55 °C were related to changes observed in
this study in the hygroscopic properties of orange, mango and prickly
pear peel. When treated at 22 °C, mango peel desorption resulted in
RWSCaw values of 0.08–0.30. Changes in orange peel desorption

51
V. Tejada-Ortigoza et al. Innovative Food Science and Emerging Technologies 43 (2017) 45–53

Fig. 3. Effect of 600 MPa and 10 min treatment on the re-

lative water sorption changes for A) adsorption and B) des-
4.0 Mango 22°C Mango 55°C
Orange 22°C Orange 55°C A orption isotherms of orange, mango and prickly pear peel
modelled with Peleg equation.
3.5 Prickly pear 22°C Prickly pear 55°C

3.0

2.5
RWSCaw

2.0

1.5

1.0

0.5

0.0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
-0.5

-1.0
aw

8.0 Mango 22°C Mango 55°C

Orange 22°C Orange 55°C B
Prickly pear 22°C Prickly pear 55°C
7.0

6.0

5.0
RWSCaw

4.0

3.0

2.0

1.0

0.0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
-1.0
aw

reached RWSCaw values of 7.5 and 5.9 when treated at 55 and 22 °C,
respectively. HHP treatment at 55 °C increased the adsorption EMC of
prickly pear peel resulting in RWSCaw = 1.1. HHP treatment produces
fruit fibers with greater capacity to retain water which may improve
food formulation applications.
Acknowledgments
The Authors acknowledge the support from Tecnológico de
Monterrey (Research Chair Funds GEE 1A01001 and CDB081) and
México's CONACYT Scholarship Program (Grant Nos. 260692 and
205265) and Project CB2014-237271.
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