Carbohydrate Polymers 179 (2018) 282–289

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Carbohydrate Polymers
journal homepage: www.elsevier.com/locate/carbpol

Pectin from Husk Tomato (Physalis ixocarpa Brot.): Rheological behavior at MARK
different extraction conditions
Blanca E. Morales-Contrerasa, Walfred Rosas-Floresa, Juan C. Contreras-Esquivelb,
⁎
Louise Wickerc,d, Juliana Morales-Castroa,
a
TECNM/Instituto Tecnológico de Durango, Blvd. Felipe Pescador 1803, Nueva Vizcaya, 34080 Durango, Dgo., Mexico
b
Universidad Autónoma de Coahuila, Facultad de Ciencias Químicas, Ing J. Cárdenas Valdez, República, Saltillo, Coah., Mexico
c
School of Nutrition and Food Sciences, Louisiana State University, Agricultural Center, Baton Rouge, LA 70808, USA
d
Department of Food Science and Technology, University of Georgia, Athens, GA 30602-7610, USA

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

Keywords: A rheological study was carried out to evaluate formulations of test dispersions and gels of high methoxyl pectins
Physalis ixocarpa Brot (HTHMP) obtained at different conditions from husk tomato waste (Physalis ixocarpa Brot.). The effect of ex-
Rheology traction agent (hydrochloric acid or citric acid), blanching time (10 or 15 min) and extraction time (15, 20 or
Husk tomato 25 min) on the rheology of the tested samples was evaluated. Flow behavior and activation energy were eval-
Pectin
uated on the test dispersions, while (Ea) frequency sweeps, temperature sweep, creep-recovery test and pene-
Tomatillo
Gels
tration test were performed on the gels. HTHMP dispersions showed shear thinning flow behavior, while
showing a good fit to Cross model. Extraction agent, blanching time and extraction time did not have effect on
Cross parameters (ηz, η∞, C, and m). Ea decreased as blanching time and extraction time increased. Frequency
sweeps revealed high dependence on frequency for both G’ and G”, while temperature sweeps (25- 95 °C)
showed thermostable husk tomato pectin gels. Hydrocloric acid (HCl) extracted pectin gels showed stronger
structure than citric acid (CA) gels.

1. Introduction
Pectins are one of the most sought out ingredients in the food in-
dustry for their unique gelling capacity and health benefits; as a result,
they have become extensively used as gelling, stabilizing, thickening,
and texturizing agents (Nascimento, Simas-Tosin, Iacomini,
Gorin, & Cordeiro, 2016). In addition, health benefits of pectins as so-
luble fibers, have been reported: control of cholesterol level, improve-
ment of gastrointestinal functions, and, preventive properties in dis-
eases such as diabetes, obesity, coronary heart diseases and certain
types of cancer (van der Gronde, Hartog, van Hees, Pellikaan, & Pieters,
2016; Wicker & Kim, 2016; Zhu et al., 2015).
Pectins, as substances of vegetal origin, are complex hetero-
polysaccharides composed of three main domains: one “lineal domain”
corresponding to homogalacturonan (HG), and, two “branched do-
mains” corresponding to rhamnogalacturonan I (RG-I) and rhamnoga-
lacturonan II (RG-II) (Morris, Ralet, Bonnin, Thibault, & Harding,
2010). HG is the most abundant pectic component, it consists of units of
D-galacturonic acid (α-1,4-linked) which can be methoxylated at C6
and/or acetylated at C2 or C3. (Cameron, Kim, Galant, Luzio, & Tzen,
2015).
Pectins are classified into two groups according to their DE: Low
Methoxyl Pectin (LMP) and High Methoxyl Pectin (HMP), with a pro-
portion of methoxyl groups lower and greater than 50%, respectively
(Fishman et al., 2015). The gelation mechanism in LMP is mediated by
the formation of calcium bridges between two carboxyl groups from
two chains in close contact, specifically, in an interaction described by
the “egg box” model (Axelos & Thibault, 1991). In HMP, junction zones
are stabilized by a combination of hydrogen bonds and hydrophobic
interactions between pectin molecules (Oakenfull, 1991). Both LMP and
HMP, can form gels under different conditions with wide characteristics
(Löfgren, Guillotin, & Hermansson, 2006), which expands their poten-
tial applications (Löfgren & Hermansson, 2007). Chemical composition
of pectin expressed by DE, molecular weight (MW) and neutral sugars
composition, have a major role in their rheological behavior
(Axelos & Thibault, 1991), thus influencing their possible uses
(Morris & Ralet, 2012).
Commercially, pectin production is mainly obtained from agro-in-
dustrial by-products from juice processing, apple pomace and citrus
peels. However, since the applications of this polysaccharide have been

⁎
Corresponding author.
E-mail address: jmorales@itdurango.edu.mx (J. Morales-Castro).

http://dx.doi.org/10.1016/j.carbpol.2017.09.097
Received 7 July 2017; Received in revised form 26 September 2017; Accepted 28 September 2017
Available online 29 September 2017
0144-8617/ © 2017 Elsevier Ltd. All rights reserved.
B.E. Morales-Contreras et al.
expanding over time, continuous research to explore and analyze other
botanical sources of extraction is currently being performed. Global
market estimations of pectin demand have been steadily increasing
over 4% annually since 2011 (above 30,000 tons, annually), indicating
a deficit in pectin production since its total production capacity only
reaches 45–50 Mton per year, (Valdés, Burgos, Jiménez, & Garrigós,
2015).
Husk tomato fruit (Physalis ixocarpa Brot.) or tomatillo, is originated
in Mexico and it is currently harvested in many other countries as a
vegetable crop. This fruit is used as a culinary ingredient in the pre-
paration of many sauces due its thickening capacity and distinctive
flavor, both in raw and cooked form (Zhang, Khan, Bakht, & Nair,
2016). Despite its wide use as food ingredient, a lack of knowledge
exists on the thickening properties of husk tomato that have not been
previously reported and some studies were conducted at our laboratory
to address this issue. Besides, significant amounts of husk tomato are
daily wasted in markets due a lack of refrigerated storage, oversupply
(year-round crop production in Mexico) and short shelf-life. Even with
the lack of available data on tomatillo waste generated in Mexico, it was
evident from on-site visits and personal interviews with distributors,
that such wastes are considerable (10–40%). Therefore, the potential of
tomatillo waste as source of pectins was explored. High methoxyl
pectins from husk tomato were extracted and physicochemically char-
acterized (Morales-Contreras, Contreras-Esquivel, Wicker, Ochoa-
Martínez & Morales-Castro, 2017). The extraction conditions tested
(blanching and extraction time) affected the physicochemical proper-
ties: Molecular weight, MW, (542–669 kDa), uronic acid content, AUA
(59.5–77.4%), degree of methylesterification, DE, (63.4–91.6%) and
the neutral sugar composition: rhammose, arabinose, galactose, fucose,
glucose, and xylose. The yield of extraction ranged from 9.6 to 19.8%.
As observed, extraction conditions determined the quality of the ob-
tained pectin from husk tomato. Regarding functional properties, pectin
is considered a rheology modifier that allows to achieve desirable flow
characteristics such as thickening food matrixes, gelling behavior and
texture, which affect sensory acceptability, stability and overall quality
of the product (Chan, Choo, Young and Loh, 2017; Herbstreith & Fox,
2015). Subsequently, it is necessary to study pectin dispersions and
gels, on the rheological and gelling properties obtained under different
extraction conditions, besides other reasons: 1) To have a reliable test
that evaluates gel strength; 2) Rheological measurements can be used to
strengthen information of internal structure of a gel obtained from
other techniques: 3) Instrumental measurements may be used instead of
sensory methods for the evaluation of texture of food gels (Gross,
Rao, & Smit, 1980). Accordingly, once the physicochemical properties
were determined (Morales-Contreras et al., 2017), the rheological be-
havior of husk tomato waste pectin was required to provide information
on the gel type and gelification mechanism for potential applications.
Therefore, the present study seeks to evaluate the effect of extraction
conditions on the rheological behavior of husk tomato pectin disper-
sions and properties of the formed gels under appropriate conditions.
2. Experimental
2.1. Materials
Husk tomato (Physalis ixocarpa Brot.) waste “Rendidora” variety
was the raw material for pectin extraction. Blanching of husk tomato
was performed in an electric steamer (T-fal Fn4 Tefal Steam Cuisine).
Extraction agents were hydrochloric acid (7647-01-0 EMD), citric acid
(77–92–9 JT.Baker). Precipitating agents were ethanol 96% (64-17-5
Hycel), and acetone (67-64-1 Macron Chemical). Solutions and gels
were prepared with calcium chloride (75-15–0 JT.Baker) and brown
sugar (Zulka, Mexico).
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Carbohydrate Polymers 179 (2018) 282–289
2.2. Extraction of husk tomato high methoxyl pectin (HTHMP)
Pectin extraction process from husk tomato waste (Physalis ixocarpa
Brot.) was previously described by Morales-Contreras et al. (2017) with
a slight modification in the extraction agents. Briefly, husk tomato was
blanched at two times (10 and 15 min); acid hydrolysis was conducted
using 1% of citric acid and 0.1 N of hydrochloric acid in a 1:3 ratio
(dried husk tomato/corresponding acid), at 100 °C for 15, 20 or 25 min.
Thereafter, extract was filtered (coffee filter No. 4 Melitta Sao Paulo,
Brasil), and centrifuged at 7500 x g for 30 min at 25 °C (Sorval Biofuge
primo R, Thermo Scientific, USA). To precipitate, extract was mixed
with ethanol (95%) at a 1:3 ratio, and the sample was equilibrated for
24 h at 4 °C. Samples were then washed with acetone. After filtration,
precipitate was dried at 60 °C in a tray dryer (SEM 2 Polinox City,
Mexico) for 4 h. Once dried, samples were milled and passed through a
No. 40 mesh and stored in dark containers. Pectin was characterized by
the analysis of uronic acid (UA), degree of esterification (DE), MW,
viscosity and neutral sugars, and yield of extraction calculated, as re-
ported in a previous publication (Morales-Contreras et al., 2017;
Morales-Contreras, 2015)
2.3. Rheological behavior of pectin dispersions
Husk tomato high methoxyl pectin, HTHMP at 1% (w/w) was dis-
persed in deionized water by magnetic stirring for 12 h at 25 °C. Flow
behavior of 1% HTHMP dispersions was determined at 25 °C (Wang,
Wang, Li, Xue, & Mao, 2009) using a Discovery Hybrid Rheometer 3 (TA
Instruments, USA) with a 40-mm parallel plate geometry (SST ST Sand-
Blast ARG2) and a measurement gap of 1000 μm. Before testing, sam-
ples were stabilized at 25 °C. Flow curves for all samples were evaluated
in an increasing shear rate range (50–500 s−1). Stress (σ) and viscosity
(η) were measured as a function of shear rate. Data of flow curves were
fitted following Cross model (Eq. (1)) (Cross, 1965), using Curve Fitting
Toolbox Ver. 3.5.4 from Matlab Software R2016b ver. 9.1.0.4416 (The
Mathworks, MA, USA).
ηz − η∞
η = η∞ +
1 + (Cγ˙ m) (1)
Where: ηz = zero-shear viscosity, η∞ = infinite shear viscosity,
C]Cross Characteristic Time constant, m = rate constant, and
γ̇ = shear rate.
2.4. Activation energy
In polymeric materials, like pectins, viscous flow can act as a
thermal process (González-Cuello, Ramos-Ramírez, Cruz-
Orea, & Salazar-Montoya 2012). As temperature increases, the energy
of the molecules also increases, therefore, it is possible to relate visc-
osity and temperature using the Arrhenius-like Eq. (2) and calculate
activation energy (Ea) (Rao, 2014).
Ea
η = η0 exp
RT (2)
Where: η = viscosity, η0 = pre-exponential constant, Ea = activation
energy (J/mol), R = universal gas constant (8.314 × 10−3 kJ/mol K),
and, T = temperature (K). Activation energy values were calculated
from the slope of Ea/R obtained from plotting ln η versus 1/T. Viscosity
of HTHMP dispersions (1%) was determined as previously described
(section 2.3). Measurements were performed at different temperatures
(25, 35, 45, 55 and 65 °C) and at a shear rate of 300 s−1 (Rosas-Flores,
Ramos-Ramírez, & Salazar-Montoya, 2013).
2.5. Pectin gels preparation
For viscoelastic characterization, gels were formulated based on the
methodology proposed by Sousa, Nielsen, Armangan,
B.E. Morales-Contreras et al.
Larsen & Sorensen, 2015, with some modifications as follows: 15 ml of
HTHMP dispersion (1% w/w) was prepared in deionized water by
magnetic stirring for 12 h at 25 °C to ensure complete dispersion. Next,
refined sugar was added until reaching a soluble solids content of 55%
(w/w), followed by 30 mg of CaCl2 and pH was adjusted to 2.5 by
adding citric acid. Gels were prepared at 60 °C and thoroughly mixed
using a magnetic stirrer. Later, formulations were poured into silver
rings (40-mm in diameter and 2-mm in height), placed on petri dishes
and allowed to stand for 4 h at 4 °C. Finally, gels were removed with a
spatula and loaded onto the rheometer plate for analysis.
2.6. Creep-Recovery test, frequency, and temperature sweeps of pectin gels
Small amplitude oscillatory shear tests were performed in a rhe-
ometer (the model and plate geometry were mentioned earlier in sec-
tion 2.3). Initially, strain sweeps measurements (0–100%) were carried
out in the pectin gels previously prepared (section 2.5.) to determine
the linear viscoelastic region at constant frequency of 10 rad/s and
25 °C. Thereafter, a strain of 0.01% within the linear viscoelastic re-
gion, was selected for frequency and temperature sweeps. During fre-
quency sweeps, storage modulus (G’) and loss modulus (G”) were
monitored in a range of 10−1 to 102 rad/s of angular frequency at
25 °C. For temperature sweeps, G’ and G” were determined as a function
of temperature (25 °C to 95 °C) with a heating rate of 5 °C/min, at a
frequency of 10 rad/s. A creep-recovery study was conducted, where
the pectin gels were subjected to a stress of 1.0 Pa at 25 °C during 180 s;
once the stress was removed, measurements were performed. Creep
curves were analyzed according to Burgers model with one Kelvin-Voigt
element (Eq. (3)) (Steffe, 1996). Curve Fitting Toolbox 3.5.1 of En-
vironment Matlab Software R2016b ver. 9.1.0.4416, was used (The
Mathworks, MA, USA).
−t ⎞ ⎞ t higher concentrations of pectin solution (2%), shear thinning behavior
J = J0 + J1 ⎛⎜1 − exp ⎛ ⎜ ⎟ +
⎟
⎝ ⎝ λret ⎠ ⎠ μ 0 (3)
Where: J = compliance, t = time, J0 = instantaneous compliance,
J1 = retarded compliance, λret = retardation time of Kelvin-Voigt ele-
ment, and, μ0 = Newtonian viscosity of free dashpot.
2.7. Textural analysis
Texture measurements were performed using a Texture Analyzer
(TA XTplus, Texture Technologies Corp, New York, USA) equipped with
a 5-kg load cell using a penetration test. Samples were prepared under
the following conditions: At 25 °C, 30 ml of pectin solution (1% w/w)
were placed in glass beakers (50 ml) and 37 mm diameter, refined sugar
was added until reaching a soluble solids content of 75% (w/w), pH was
adjusted to 3.0 using CA, followed by addition of 0.5 ml of CaCl2 (sa-
turated solution). Then, samples were allowed to settle for 4 h at 4 °C
for gel curing. Afterwards, samples were conditioned at room tem-
perature and loaded onto the texturometer for analysis. A cylindrical
probe of 22 mm of diameter was used at a speed of pre-test, test, and
post-test of 2 mm/s. Gels were penetrated to a depth of 20 mm.
Obtained parameters were: rupture strength, brittleness and adhesive-
ness of gels through the software of the instrument (Exponent Version
5.1.1.0) with the Macro option program.
2.8. Statistical analysis
A full factorial experimental design was used, where three factors
were analyzed: blanching time (10 or 15 min), extraction agent (hy-
drochloric acid or citric acid) and extraction time (15, 20 or 25 min).
All analyses were performed in triplicates. Data were analyzed using
one-way analysis of variance (ANOVA) followed by Fisheŕs least sig-
nificant difference (LSD). Means were considered to be significantly
different at p < 0.05. Statistical software used was Minitab version
284
Carbohydrate Polymers 179 (2018) 282–289
Fig. 1. Viscosity behavior versus shear rate for husk tomato (Physalis ixocarpa Brot.)
pectin dispersions at 1%.
17.1 (Minitab, Inc. State College, PA).
3. Results and discussion
3.1. Flow behavior of husk tomato pectin dispersions
Under adequate biopolymer concentrations, HTHMP dispersions
exhibited viscous response in three stages, when sheared over a wide
shear rate range: Zero-shear viscosity (ηz), shear-thinning range, and,
infinite-shear-viscosity (η∞). Flow behavior analyses (Fig. 1) showed
that all samples exhibited shear thinning or pseudoplastic behavior.
Such behavior is consistent with data reported by Hosseini,
Khodaiyan, & Yarmand (2016) for sour orange peel pectin, where at
was exhibited, and a similar behavior for pectin from carrot pomace
was found (Jafari, Khodaiyan, Kiani & Hosseini, 2017). Sousa, Nielsen,
Armagan, Larsen, & Sørensen (2015) revealed a comparable behavior
(shear thinning) for citrus pectin that was attributed to the physical
disruption of chain entanglements in pectin dispersions. As observed,
highest values of ηa corresponded to pectin samples extracted with ci-
tric acid at 15 and 25 min of blanching and extraction time, respec-
tively. While lowest values were obtained with hydrochloric acid at 10
and 20 min blanching and extraction time, (HCl1020) respectively.
Obtained results could be related to the low dissociation constant pre-
sent in organic acids (such as citric acid), which causes less proto-
ncatalyzed depolimerization (Oliveira et al., 2016). As citric acid was
used, pectin chains maintained their structure; molecules with higher
size and greater resistance to movement originated greater viscosity
values. Overall, higher viscosity values were obtained from samples
treated with citric acid rather than hydrochloric acid.
Experimental data of flow curves were fitted to the rheological Cross
model since apparent viscosity of dispersions can be correlated with
shear rate using this Eq. (1). The selection of this model was based on
the characteristic of pectins, considered as time independent fluids and
the Cross model has been reported to describe the behavior of time-
independent fluids (Steffe, 1996); in addition, it offers a complete
profile of viscosity vs shear stress. Moreover, other published studies
presented the use of this model in different polysaccharides in disper-
sion (pectin included) that exhibited a shear thinning behavior with a
zero-shear rate viscosity, (Babatope, 2005; Lopes da Silva et al., 1992;
Lopes da Silva, Gonçalves, & Rao,1994; Min, Bae, Lee, Yoo, & Lee, 2010;
Vriesmann, Teófilo, & Lúcia de Oliveira Petkowicz, 2012) which sup-
ports the use of this model to describe the behavior of husk tomato
pectin dispersions.
Cross model parameters are presented in Table 1. All samples had an
acceptable fit with correlation coefficients (R2) between 0.97-0.99. In
the Cross model, C represents relaxation time, also known as Cross time
B.E. Morales-Contreras et al. Carbohydrate Polymers 179 (2018) 282–289

Table 1 black currant) in the range of 32–39 kJ/mol (Bélafi-Bakó, Cserjési,

Cross-model parameters (η0, η∞, C, m) for pectin of husk tomato (Physalis ixocarpa Brot.) Beszédes, Csanádi, & Hodúr, 2012). Mohammadifar, Musavi,
solutions (1%).
Kiumarsi & Williams (2006) indicated that low values of activation
Sample η z Pa s η∞ Pa s Cs m energy indicate fewer inter and intra interactions between polymer
chains.
HCl 10/15 0.1325b,c 0.003320a 0.1841a 0.2757a,b Extraction conditions of husk tomato pectin impacted activation
HCl 10/20 0.1118c 0.000090a 0.2413a 0.2153b
energy significantly, suggesting that both blanching time and extraction
HCl 10/25 0.1914a,b,c 0.000174a 0.1255a 0.2570b
HCl 15/15 0.1743b,c 0.001480a 0.2970a 0.2903a,b time modify pectin structure and the degree of interaction between
HCl 15/20 0.1303b,c 0.000239a 0.1279a 0.2542b molecules. Statistical comparison of individual factors (HCl vs CA,
HCl 15/25 0.1655b,c 0.002400a 1.0400a 0.2481b 10 min vs 15 min of blanching time, 15 vs 20 vs 25 of extraction time)
CA 10/15 0.3275a,b 0.017530a 0.1478a 0.5615a showed no significant effects; however, when the interactions between
CA 10/20 0.2039a,b,c 0.006220a 0.1911a 0.3650a,b
factors were considered, values were significantly different.
CA 10/25 0.1719a,b,c 0.000145a 0.1543a 0.2827a,b
CA 15/15 0.2906a,b,c 0.013100a 0.2060a 0.4455a,b
CA 15/20 0.3851a 0.013730a 0.1926a 0.4580a,b
CA 15/25 0.3011a,b,c 0.002400a 0.1407a 0.3843a,b 3.3. Frequency sweeps of HTHMP gels

HCl = Hydrocloric acid; CA = Citric acid; Different letter indicate significant differences.
of the polymer in solution, being a critical parameter that describes the
end of zero-shear viscosity and the onset of shear thinning. At this
point, the movements rates acting on the fluid become greater than the
rates of formation of new entanglements, leading to a crosslink density
reduction, and, in consequence, a decrease of viscosity (Morris, Cutler,
Ross-Murphy, Rees & Price, 1981). In spite that magnitudes are appar-
ently different, statistical analysis showed no significant difference
between treatments; however, this parameter is a macroscopic re-
presentation of the microstructural nature of the polymer and it is re-
lated to the number of links and interactions between its molecules,
which depend on molar mass (Bourbon et al., 2010).
3.2. Activation energy
Since pectin solutions endure different processing conditions, their
viscosity should be studied as a function of temperature; nevertheless,
few studies are available on pectin experimental data viscosity with
temperature. Activation energy in fluids is considered as the barrier
created by surrounding building units that molecules need to overcome
to move (Rosas-Flores et al., 2013). In this research, viscosity of dis-
persions was determined at 25, 35, 45, 55 and 65 °C (298.15, 308.15,
318.15, 328.15 and 338.15 K, respectively) (Eq. (2)). Results showed
that ln η decreased linearly while increasing temperature (not pre-
sented). Such effect can be attributed to the increase of intermolecular
spaces as consequence of thermal expansion. Ea values (13.9-18.3 kJ/
mol) (Fig. 2) obtained from viscosity data at different temperatures
were below values reported for citrus pectin (25 kJ/mol) (Zhao et al.,
2015) and other pectins (apple, red currant, raspberry, elderberry and
Pectins can form gels under a broad range of conditions and factors,
such as sucrose content, calcium concentration, pH and temperature,
which have a strong influence on the rheological properties for both
LMP and HMP (Gigli, Garnier, & Piazza, 2009; Löfgren,
Guillotin, & Hermansson, 2006), although, for this research, those
parameters were kept constant. To effectively characterize mechanical
response of pectin gels, material properties like Storage Modulus
(elastic) (G’) and Loss Modulus (Viscous) (G”) were determined over a
wide range of frequencies. Conditions and formulations for the pre-
paration of these gels are specified in section 2.5. Results for some
samples are presented in Fig. 3, although the rest of the samples pre-
sented a similar response; according to Clark & Ross-Murphy (1987),
three different types of behavior can be identified from this ratio: li-
quid-like (G” > G’), concentrated solution (G” = G’) and gel-like
(G’ > G”) behavior. Accordingly, with this classification, most of husk
tomato pectin samples tested, displayed a gel-like behavior (G’ > G”),
(Fig. 3) indicating the formation of a network.
Furthermore, the mechanical response of gels revealed that both G’
and G” are highly dependent of frequency throughout the applied range
(0.1–100 rad/s). This behavior might indicate a relaxation process due
to movements of galacturonic units inside the junction zones
(Ngouémazong et al., 2012). A resembling frequency dependence be-
havior has been previously reported (Jamsazzadeh Kermani,
Shpigelman, Pham, Van Loey, & Hendrickx, 2015) for 5% mango peel
pectin solutions without transition sol-gel and for palmyra palm pectin,
where Ǵ and G” increased with frequency, indicating a continuous
network structure formation (Assoi et al., 2014). Highest G’ and G”
values were obtained from sample HCl1015 (Hydrochloric acid/10 min
of blanching time/15 min of extraction time), which corresponds to the
lowest viscosity value (section 3.1). Gels with HCl treatment, showed G’
values higher than samples treated with citric acid due the proton

Fig. 2. Activation energy of 1% husk tomato (Physalis ixocarpa Brot.) pectin dispersions. Fig. 3. Frequency sweeps for husk tomato (Physalis ixocarpa Brot.) pectin gels (Fill color
(Extraction agent/Blanching time/Extraction time). represents G’, empty color represents G”).

285
B.E. Morales-Contreras et al.
catalyzed depolymerization process, where many junction zones may
have been exposed and pectin chains interact more with calcium ions
and glucose, forming stronger systems. The acid depolymerization of
pectin, causes changes in its rheological behavior, due to the breakage
of bonds in the polygalacturonic backbone (Oosterveld, Beldman,
Schols, & Voragen, 2000; Thibault, Renard, Axelos, Roger, & Crépeau,
1993), which is evident by the decrease in molecular weight. In the
present study, we concluded that pectin depolymerization produced
stronger gels since samples treated with HCL, higher degree of poly-
merization, (average MW 611 kDa), exhibited higher values in magni-
tude of G’ than samples obtained with CA, (average molecular weight
649 kDa), as can be seen in Fig. 3, by observing the curves, where HCL
curves are above Citric Acid curves.
Otherwise, gel-sol transition point (G’ = G”) or so-called con-
centrated solution behavior, was observed with both extraction agents
at conditions of HCl1520 (Hydrochloric acid/15 min of blanching time/
20 min of extraction time) and CA1020 (Citric acid/10 min of
blanching time/20 min of extraction time). This phenomenon may
occur when molecules do not disentangle during a long period of os-
cillation at low frequencies, and their entanglement points play a role of
temporary knots of 3D network. In this way, the solution behaves as
elastic solid, whereas during a short period of oscillation at high fre-
quencies, the structure have a tendency to behave as a viscous liquid
and the molecular chains disentangle (Nishinari, 1997). In this re-
search, typical gel-like behavior (G’ higher than G”) was found for all
husk tomato pectins. Such behavior is not consistent to other reports
that used different pectin sources, where viscoelastic liquid character-
istics (G” higher than G’) were reported with palm pectins (Assoi et al.,
2014) and tamarillo fruit (Nascimento et al., 2016). Nascimento et al.
(2016) specifies that this type of behavior has been observed in pectins
from sources such as apple pomace, cacao pod husk and red tamarillo
fruit.
3.4. Temperature sweeps
Temperature is relevant in the gelation mechanism of HMP, since
hydrophobic interactions can be formed between methoxyl groups
during the cooling process. Under certain conditions, each poly-
saccharide has a melting temperature “Tm”. If a thermo-reversible
structure is going to be formed, temperature plays an important role on
gel stability, affecting rheological parameters such as G’ and G”. Along
this line, temperature sweep studies were conducted (25–95 °C) to de-
termine G’ and G” as a function of temperature at constant frequency
(10 rad/s) to identify any thermo-reversibility of gels formed. For all
samples, G’ and G” increased as temperature increased; Fig. 4 shows
two representative extracted samples: one treated with HCl and the
other with CA. Remaining samples presented similar behaviors. Results
showed that HTHMP gels, did not present thermo-reversibility
Fig. 4. Temperature sweeps for husk tomato (Physalis ixocarpa Brot.) gels.
286
Carbohydrate Polymers 179 (2018) 282–289
characteristics. Since G’ and G” did not intersect at any point (Gel-Sol
behavior in function of temperature), it can be assumed that a melting
point does not exist, thus a melting temperature was not found. It is
known that thermo-reversibility phenomena is present when hydrogen
bonds maintain the pectin network structure, mainly by the interaction
between charges from water molecules and polysaccharides. Once the
system is heated, absorbed energy causes water molecules to move
faster, pectin gel structure is lost, and, consequently, it returns to the
dispersion state. This behavior is characteristic of High Methoxyl Pec-
tins. On the other hand, a lack of thermo-reversibility phenomena oc-
curs when the network structure is maintained by charges between
cross linkers (such as Ca2+) and negative charges present in pectin. In
this type of structures, water is trapped inside providing volume and
plasticity. When the system is heated, water molecules break away and
gel volume decreases significantly due to water loss and an increment of
G’ and G” magnitudes, which is characteristic of LMP.
Since husk tomato pectin was classified as High Methoxyl Pectin
(HMP) with a DE between 63 and 91% (Morales-Contreras et al., 2017),
and the non-thermo-reversibility property is characteristic of Low
Methoxyl Pectin (LMP), a contradiction arises from these results;
however, Calcium-Sensitive Pectins (CSP, classified as HMP) can form
gels in the presence of calcium, as long as blocks of de-esterified pectin
are present (Hotchkiss et al., 2002). This description has a resemblance
to the characteristics of HTHMP, where Ca2+ was needed to form gels;
based on this, HTHMP might belong to this category, as CSP; Overall,
temperature did not show an influence on G’ and G” values to induce a
sol-gel transition.
In food technology, the design and control of gel microstructure is a
key parameter to ensure consumer satisfaction in many food products,
such as yoghurt, cheese, pudding, sausage, and tofu (Joshi, Aldred,
Panozzo, Kasapis & Adhikari, 2014). Non-thermo- reversible gels are
preferred since they may be formed and processed at higher tempera-
tures and remain stable over time (Brenner, Nicolai, & Johannsson,
2009).
3.5. Creep-Recovery test
The slow deformation of samples held under constant shear stress
testing, allows to measure small molecular motion in a more precise
manner than through oscillatory testing. In a Creep-Recovery test, an
instantaneous stress is applied to the pectin gels and once the stress is
removed, changes are registered over time, where some recovery may
be detected, as the material attempts to return to its original shape
(Dolz, Hernández, & Delegido, 2008). In Fig. 5, Creep-Recovery profile
was plotted (%γ vs Time) for two representative HTHMP samples. All
samples displayed a true viscoelastic behavior. The nonlinear response
to strain and the ability to recover some structure by storing energy,
Fig. 5. Creep-Recovery behavior of husk tomato (Physalis ixocarpa Brot.) pectin gels.
B.E. Morales-Contreras et al. Carbohydrate Polymers 179 (2018) 282–289

Table 2
Burgers model constants and recovery percentage for husk tomato (Physalis ixocarpa
Brot. pectin gels.

Samples Burgers Model Parameter Recovery

J0 (Pa−1) J1 (Pa−1) λret (s) μ0 (Pa.s) R2 (%)

HCl 10/15 0.0499 0.5445 0.1000 0.0022 0.8931 70

HCl 10/20 0.5032 1.0861 0.8831 0.0057 0.9286 33
HCl 10/25 0.5034 1.0859 0.8843 0.0057 0.9286 58
HCl 15/15 0.0830 0.2440 0.3038 0.0017 0.9378 81
HCl 15/20 0.6749 9.8950 0.8175 0.0267 0.9662 53
HCl 15/25 0.1624 1.4435 0.3217 0.0037 0.9433 73
CA 10/15 0.0930 0.9097 0.1000 0.0034 0.8996 29
CA 10/20 0.8621 6.8250 1.129 0.0243 0.9627 43
CA 10/25 0.2782 0.7446 0.4403 0.0037 0.9029 68
CA 15/15 0.0870 0.5923 0.7264 0.0025 0.9639 55
CA 15/20 0.6914 3.2661 1.0070 0.0113 0.9443 72
CA 15/25 0.2143 0.4488 0.6658 0.0023 0.9263 51

confirmed a permanent deformation, below the total deformation ap-
plied to the sample (Steffe, 1996). Kelvin model shows good elastic
retardation; however, it is limited to analyze biological materials.
Nevertheless, Burgers model offers a better fit for the materials used for
this research, since it is based on Kelvin and Maxwell models and both
consider elastic and viscous components in series, i.e., as if they oc-
curred at the same time. At the beginning of creep testing, a change in
the compliancy is recorded, which is instantaneous (J0), due the spring
component in Maxwell’s model. Then, an exponential change in com-
pliance can be observed, which relates to the retardation time (λret),
and, finally, the independent dashpot that describes viscous response.
Burgers model constants are shown in Table 2. Sample HCl1015 (hy-
drochloric acid/10 min of blanching time/15 min of extraction time)
displayed the lowest value for J0, whilst sample CA1020 (citric acid/
10 min of blanching time/20 min of extraction time) presented the
highest value. J0 represents an instantaneous change in compliance to
the spring in the Maxwell component of Burgers model and can be
expressed as the pure elastic response of the material. Highest values
registered for retardation time (λret) corresponded to citric acid ex-
tractions (CA1020 and CA1520), while lowest corresponded to hydro-
chloric acid extraction (HCl1015). This parameter is unique for each
substance, and in viscoelastic materials, it describes the time where a
maximum strain is achieved. Independent dashpot causes a permanent
deformation in the material, i.e., that fraction that can not be re-
covered, deformation that is expressed as the recovery percentage,
which describes the magnitude of recovery of the studied system (gels),
when the stress is removed, an instantaneous change in compliance
occurs and the free dashpot causes a permanent deformation in the
material that is directly related to the non-recoverable sample strain.
Eq. (4) (Dolz et al., 2008), allows to calculate the percentage of re-
covery:
J − Jmin ⎞
%REC = ⎛ max⎜ *100 ⎟
Fig. 6. Radar plot for textural parameters for husk tomato (Physalis ixocarpa Brot.) pectin
gels.
in pectin that are evidenced in this research through the obtained re-
sults of recovery percentage, which is an indirect measure of gels
elasticity.
3.6. Penetration test
Textural attributes are key factors for consumer acceptance in food
quality and are influenced at molecular level by the interactions be-
tween macromolecules in the structured matrix (Pereira, Singh,
Munro, & Luckman, 2003). In Fig. 6, rupture strength, brittleness and
adhesiveness are shown in a radar plot; results showed that the max-
imum value obtained for rupture strength was 542.52 gf for HCl1525
and the minimum one was registered for CA1015 with 48 gf. By com-
paring these values with other conventional sources of pectin, such as
orange or lemon peel (183 gf and 250 gf, respectively, Sousa et al.,
2015), husk tomato pectins are below and above these values, due
different conditions in the extraction process. Rupture strength is the
maximum force supported by the gel structure before collapsing, and it
indicates how strong the gel really is (Fishman & Cooke, 2009). In this
sense, obtained gels from HCl extracted pectin showed a stronger
structure than gels obtained using CA, as seen in Fig. 6, where the larger
area is in HCl side of the plot. Gel brittleness is obtained from the
distance that the probe penetrates before the rupture occurs, which
means that at shorter distance, the more brittle the gel is (Genovese,
Ye, & Singh, 2010). Greatest brittleness was obtained from CA1020,
with a penetration distance before gel rupture of 27.06 mm, while
lowest brittleness was HCl1015 with 38.54 mm. Adhesiveness can be
described as the total force (area under the negative region of the
curve) recorded when the probe is removed (Genovese et al., 2010).

⎝ Jmax ⎠ (4)
Recovery percentages of all the analyzed samples are shown in
Table 2. Highest recovery value was obtained from HCl1515 sample
(81%), while the lowest corresponded to CA1015 sample (29%). An
average of recovery percentage was determined and contrasted be-
tween CA and HCl samples. Pectin gels extracted with HCl presented
the highest values (61.33%) of recovery percentage, while gels ex-
tracted with CA exhibited lower values. In this way, HCl extracted
pectins gels were more capable to return to their original shape that the
ones formed with pectin extracted using CA. Obtained results suggest
that HCl extracted pectin generated gels more elastic than the ones with
pectins obtained through CA. An effect of the extraction agent on the
structure of the pectin gel and its properties was observed. HCl favors
proton catalyzed depolymerization process, causing structural changes
The sample with the highest adhesiveness value was HCl1020 with
−293.59 gsec and the minimum value was obtained from CA1015 with
−59.87 gsec. Adhesiveness can be considered as the necessary work to
overcome the attractive forces between the surface of the pectin gels
and a specific surface (geometry employed), and it is related to the
breaking of cohesive bonds (Bonacucina, Cespi, Misici-Falzi, & Palmieri
2006). Obtained differences are attributed to the extraction conditions
that had an impact on the molecular structure of husk tomato pectins,
since previous studies have reported that the structure of pectin plays a
fundamental role in the textural properties of pectin gel matrixes (Kim,
Yoo, Kim, Park, & Yoo, 2008). Extracting agent (HCl or CA) has the
main impact on textural characteristics of HTHMP gels.

287
B.E. Morales-Contreras et al.
4. Conclusion
Pectin extraction agents, have a significant impact on the physical
behavior of husk tomato pectin, as evidenced by rheological behavior
for both flow test and viscoelastic tests, that suggest a structure mod-
ification depending on the tested agent. HTHMP gels, behaved like
“weak” gels due to their dependency on frequency in the analyzed
range. In addition, temperature sweeps showed non-thermo-reversi-
bility of husk tomato pectin gels with a behavior like CSP, suggesting
that structure is mainly maintained by the interaction between poly-
saccharides and cross linkers (Ca2+). Penetration test showed that
stronger gels were obtained with HCl than with CA. Obtained results
could lead to potential applications of husk tomato pectins in foods
formulations.
Acknowledgements
The authors appreciate the funding provided by Tecnológico
Nacional de Mexico, TecNM, through Grant Number 5556.15-P, and the
Scholarship No. 340864, from the National Council of Science and
Technology, CONACYT, Mexico, granted to Blanca E. Morales Contreras
to purse MSc studies.
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