International Journal of Biological Macromolecules 91 (2016) 106–114

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International Journal of Biological Macromolecules

journal homepage: www.elsevier.com/locate/ijbiomac

Analysis of the pasting profile in corn starch: Structural,

morphological, and thermal transformations, Part I
Natalia Rincón-Londoño a , Lineth J. Vega-Rojas b , Margarita Contreras-Padilla c ,
A.A. Acosta-Osorio d , Mario E. Rodríguez-García e,∗
a
Posgrado en Ciencias e Ingeniería de Materiales, Centro de Física Aplicada y Tecnología Avanzada, Universidad Nacional Autónoma de México, Campus
Juriquilla, Querétaro, Qro, C.P 76230, Mexico
b
Posgrado en Ciencias Químico Biológicas, Facultad de Química, Universidad Autónoma de Querétaro, Cerro de las Campanas S/N. Centro Universitario, C.P
76010 Querétaro, Qro, Mexico
c
División de Investigación y Posgrado, Facultad de Ingeniería, Universidad Autónoma de Querétaro, Centro Universitario, C.P. 76010 Santiago de Querétaro,
Qro, Mexico
d
CONACYT Reseearch Fellow, Tecnologico Nacional de México, Instituto Tecnologico de Veracruz, Veracruz, Ver., Mexico
e
Departamento de Nanotecnología, Centro de Física Aplicada y Tecnología Avanzada, Universidad Nacional Autónoma de México, Campus Juriquilla,
Boulevard Juriquilla No. 3001 C.P. 76230, Juriquilla, Querétaro, A.P. 1-1010, Mexico

a r t i c l e i n f o a b s t r a c t

Article history: This work is focused on the understanding of the apparent viscosity profile of corn starch, in terms of the
Received 9 December 2015 physicochemical and morphological changes that take place during the thermal profile of starch-water
Received in revised form 12 May 2016 suspension to its respective gel formation. A mathematical model was used to obtain the experimental
Accepted 18 May 2016
operating conditions that satisfy the Froude number. Freeze drying samples are studied in different stages
Available online 19 May 2016
along the pasting profile. Changes in the structural properties of the samples are studied using X-ray
diffraction, and the morphological changes are followed using scanning electron microscopy, differential
Keywords:
scanning calorimetry was used to analyze the thermal changes in starch. The changes in the pasting
Gelatinization
Pasting
profile are associated with structural, thermal,and morphological changes of the system and the analysis
Starch of the physicochemical transformation that occur during the pasting profile are explained. The finding in
Retrogradation this work does not show evidence of gel retrogradation at the end of the cooling process.
© 2016 Elsevier B.V. All rights reserved.

1. Introduction erties. Pasting properties are often obtained by studying a pasting

Starch is possibly the most important carbohydrate in mod-
ern human life, with different applications in industries such as
the food, petroleum, pharmaceutical, paint, and cosmetic indus-
tries, among others. Starch is a granule or particle composed of two
macromolecules: amylose and amylopectin [1,2]. Amylose has a
linear structure of d-glucan units bonded together by ␣-(1,4) bonds,
in the shape of a helix which consists of six fragments of glucose
per turn [3]. On the other hand, amylopectin is a branched polymer
that is composed of linear chains with ␣-(1–4) bonds and ␣-(1–6)
bonds. Amylopectin structure consists of short chains forming dou-
ble helices.
One of the most important aspects to study in the case of starch
and its derivative products are the rheological and pasting prop-
∗ Corresponding author at: Departamento de Nanotecnología, CFATA, UNAM,
Querétaro, Qro, Mexico.
E-mail address: marioga@fata.unam.mx (M.E. Rodríguez-García).
profile of a starch-water suspension, as a function of the time and
temperature. The importance of characterizing the starch past-
ing profile is that many foods containing starch are cooked with
water; this process causes great changes in the structure and mor-
phology of the starch granules [4]. These changes result in some
modified properties of the final product. Moreover, the swelling of
the starch granules during cooking begins predominantly in amor-
phous regions [5]; this property is important because it allows the
development of gel.The increase of apparent viscosity in starch-
water suspensions occurs mainly due to the exudate products
released from the starch granules forming a network [6]. There-
fore, the effects of the thermal profile and the shear rate on the
physicochemical properties of the starch-water suspension were
not studied.
Wajira and and David [7] studied the gelatinization process of
different native starches, using SEM, DSC, and X-ray diffraction
followed by the micro, thermal, and structural transformations
of starch-water suspension subjected to heating (35–85 ◦ C at 5 ◦ C

http://dx.doi.org/10.1016/j.ijbiomac.2016.05.070
0141-8130/© 2016 Elsevier B.V. All rights reserved.
 N. Rincón-Londoño et al. / International Journal of Biological Macromolecules 91 (2016) 106–114
Fig. 1. (A) and (B) SEM images of isolated corn starch, (C) shows the DSC thermogram and (D) the characteristic X-ray diffraction pattern.
intervals). Their results showed that the gelatinization is not only
an order-disorder transition between the amylose/amylopectin
arranged inside the starch granule, but the disordered system can
include the exudation of macromolecules. However, the pasting
profiles of different starches and their morphological and structural
changes as a function of the time during a pasting profile were not
studied.
There are usually five sample characteristics, which are obtained
with a pasting profile: peak viscosity and peak viscosity temper-
ature; the ease of cooking; the paste stability or resistance to
breakdown; setback or cold paste viscosity, and stability of the
cooked paste. Additionally, the setback value may indicate the ret-
rogradation tendency of the starch paste by part of components
leachate [8]. However, these definitions were only phenomenologi-
cal and no evidence of the physicochemical changes or the influence
of these changes during a pasting profile, were reported. In the same
direction, Karim et al. [9] defined the setback as the rapid retrogra-
dation of leached amylose in the starch paste, but no evidence of
the recrystallization (retrogradation) of amylose was reported.
The commercial system used to study pasting profiles is based
on the principle given by the Rushton [10] equations, about the use
of an impeller to study the rheological properties of a system. The
basic viscometer impeller assumption is that the shear rate is inde-
pendent of the rheological properties of the fluid. The experimental
system can convert the torque reading into a shear stress/shear rate
relationship.
In all the works above, even in an important number of
researches related to the pasting properties of starches, it is not
clear what kind of physicochemical changes take place during the
107
pasting profile. There does not exist a detailed explanation of the
changes in the morphology of the starch-water system as a result
of the temperature and shear rate.
The objective of this work is to explain in detail the pasting pro-
file of corn starch-water suspensions based on the physicochemical
and morphological changes that take place during the thermal pro-
file at the constant shear rate. For these experiments, corn starch
was used. The Froude number (Fr = 1) was used to determine the
experimental shear rate to carry out a pasting profile. Fr = 1 avoid
precipitation of the starch granules because at this point gravity
and inertia forces are equal. The morphological changes that take
place along the pasting profile were studied using SEM with frozen
samples; structural changes and thermal profiles were studied by
means of X-ray diffraction and DSC respectively, for different points
of the pasting profile.
2. Material and methods
2.1. Materials
Corn starch from Newport Scientific Pty Ltd. (part number
102102, Warriewood, Australia) was used in all experiments (see
Fig. 1(A) and (B)). This regular starch contains 66% of amylopectin
and 34% of amylose. Starch is characterized by a polyhedral
morphology and some spherical granules between 4–12 ␮m. The
chemical composition of the corn starch was the follows: the pro-
tein content was 0.67 ± 0.05%, fat content was 0.15 ± 0.02%, and
fiber was not detected. The characteristic Tg of this starch was
70.51 ◦ C (see Fig. 1(C)) the beginning of the thermal transforma-
108 N. Rincón-Londoño et al. / International Journal of Biological Macromolecules 91 (2016) 106–114
Fig. 2. (A)–(C) Characteristic pasting profile of isolated corn starch as well as the
first and second derivative used to determine the critical points.
Fig. 3. Pasting profile and conventional definitions used in the analysis.
tion defined as To was 64.65 ◦ C and the end of this transition was
determined at 75.64 ◦ C (Te ). While the characteristic X-ray pattern
(Fig. 1(D)) shows a semi-crystalline phase A-type amylose reported
in the Powder Diffraction File (PDF#43-1858 [11]).
2.2. Measurement of pasting profile
The pasting profiles of the starch aqueous suspensions were
determined using a rheometer model MCR 102(Anton Paar, St
Albans, United Kingdom). The starch is adjusted to 12% moisture
content and 3 g of starch and 18 ml of distilled water were used.
The thermal profile shown in Fig. 2(A) was used. Initial tempera-
ture of the system was 50 ◦ C, and it remained constant for 1 min.
The sample was then heated for 5.3 min from 50 ◦ C to 90 ◦ C, and
then held at a constant temperature of 90 ◦ C for 5.3 min. The sam-
ple was cooled down to 50 ◦ C in 5.3 min, then this temperature was
kept constant for 1 min, and 193 rpm was used.
A typical pasting profile was used to study the physicochemical
changes that take place during the thermal profile (see Fig. 2(A)).
Critical points for this profile can be determined by using the first
and second derivative criteria (see Fig. 2(B) and (C)). The deriva-
tive gives direct information about the drastic changes between
dependent (apparent viscosity) vs independent variable (time). The
pasting profile is divided into three regions: Region I corresponds
to the heating process of the starch-water suspension from 50 to
90 ◦ C; Region II corresponds to the isothermal (90 ◦ C), and region III
corresponds to the cooling (from 90 to 50 ◦ C). In these three regions
9 points along pasting profile were studied.
For region I, 4 points were studied. In order to obtain Point 1, a
pasting profile was carried out from 0 to 200 s; for point 2 pasting,
profile was carried out from 0 to 266 s; for point 3 from 0 to 285 s
that reveals changes in the first and second derivate; Point 4 from
0 to 339 s (peak viscosity). Region II corresponds to the isothermal
section of the pasting profile. By direct inspection of the first and
second derivative no changes occur in this region. Two points in
this region were studied: points 5 and 6, in which the so-called
breakdown is located. Region III corresponds to the cooling of the
pasting profile and no significant changes in the first and second
derivative were observed, also three points in these regions were
studied in order to determine the factors that influence the increase
in the viscosity as result of the cooling process (points 7–9) (See
Fig. 2(A)).
When the sample reaches each point, the rheometer is immedi-
ately stopped, and the sample is cooled in liquid nitrogen and stored
in a freezing container to avoid any change in its physicochemi-
cal properties. The samples were immediately freeze-dried using
a freeze dry Free zone 2.5 (Labconco, Kansas City, USA), for 48 h.
All samples are dried for the same time under the same thermal
conditions.
2.3. Scanning electron microscopy (SEM)
The changes in the morphology of the samples obtained for
points 1–9 of the pasting profile were analyzed by SEM, Model
JSM-6060LV at high vacuum (JEOL, Tokyo-Japan). The samples
were fixed on an aluminum specimen holder with double graphite
tape and gold coated for sputtering. The analysis was performed
employing a 5 kV electron acceleration voltage, to avoid any dam-
age of the sample due to power beam.
2.4. Differential scanning calorimetry (DSC)
The DSC thermograms of the samples obtained for points
1–9 along the pasting profile were measured using the Differ-
ential Scanning Calorimeter DSC 1 (Mettle Toledo, Greifensee-
Switzerland) and data was processed with TA Instrument software.
Calibrations were performed using pure indium. Samples of
2.0 ± 0.1 mg were prepared by adding deionized water to the sam-
ples into the pan until they reach a moisture of 85% (w/w). The
pans were hermetically sealed and kept at room temperature for
6 h. The samples were scanned from 30 ◦ C to 110 ◦ C at 7.5 ◦ C/min.
Each experiment was conducted in triplicates.
2.5. X-ray diffraction
In order to study the structural changes that take place along
the pasting profile (9 points), dry samples were studied using X-ray
diffraction. The samples were ground using a coffee miller (Krups-
USA) and then were passed through a 250 ␮m screen. The X-ray
diffraction patterns were recorded on a diffractometer (Rigaku-
Miniflex, Texas-EE.UU) operating at 35 kV and 15 mA, with a CuK␣
 N. Rincón-Londoño et al. / International Journal of Biological Macromolecules 91 (2016) 106–114 109

]
Fig. 4. SEM images of the morphological changes for region I (points 1–4) for pasting profile of isolated corn starch.

radiation wavelength of 1.5406 Å. The measurements were made where, ␩ is the Viscosity (Pa s−1 ), Pis Power consumption of the
from 5◦ to 60◦ on a 2␪ scale with a step size of 0.05. motor (W), c is a constant that depend of impeller dimensions, N is
the impeller speed (s−1 ), and D is the impeller diameter (m).
This viscometer is based on Rushton-turbine model. Rushton
3. Calculation: mathematical model for pasting profiles
et al. [10] developed this turbine from dimensionless number the-
ory and pi-Buckingham theorem. The result of both (theory and
In order to understand the physicochemical changes that take
theorem) can be written:
place during a pasting profile of corn starch, it is very important to
know the mathematical model that allow an instrument to deter- c
P0 = Fr (2)
mine a pasting profile. The viscosity measurements of mycelia Re
suspensions system must be obtained with an impeller viscometer where Po is power number, Fr is Froude number, and Re is a
system, given by: Reynolds number, given by:

P P
= (1) P0 = (3)
cN 2 D3 N 3 D5
110 N. Rincón-Londoño et al. / International Journal of Biological Macromolecules 91 (2016) 106–114
ND2
Re =
 between the swollen granules and the leachate polymers [8,16,17].
where ␳ is a density (kg m−3 ), by replacing Eqs. (3) and (4) in Eq.
(2) is possible to find ␩ (Eq. 1).
Eq. (2) is valid only if the flow isof the laminar regimen and the
Froude number (Fr) is one [10]. The Froude number is given by:
N2D
Fr =
g
where g is gravity acceleration (ms−2 ).
When the Fr number is lower than 1, the gravity forces possess
the system and whole system is not mixed; when the Fr number is
bigger than 1, the centripetal forces dominate the system and the
fluid tends to flow out of the vessel. The final option is when the
Fr number equals 1. In this case, the centripetal and gravitational
forces are equal and the system is mixed homogeneously [12].
A unique impeller velocity to carry out any experiment is set.
The pasting profiles were carried out on the Anton-Paarrheo meter
with starch cells; this device has a different geometry and, as a
result, it is necessary to calculate the impeller speed. The impeller
diameter (D) is 24 mm, g = 9.81 ms−2 , and the Fr = 1, replacing in
equation 5 obtain:
 
Frg 1 × 9.81 × 3600
N= = = 193rpm
2D 22 × 2 × 0.024
when the impeller velocity is 193 rpm, the entire system is in move-
ment and the energy is used only for this purpose. It is clear that the
system can work at any RPM, but there exists a unique frequency
in which the pasting profile makes sense physically.
4. Some definitions about starch and its changes during a
pasting profile
Before studying the physicochemical changes that take place
during a pasting profile, it is necessary to know the definitions
that describe some phenomena that take place during the thermal
process.
Gelatinization: when starch (amylose–amylopectin) is heated in
presence of water, it undergoes an order-disorder phase transition
called gelatinization. This transition occurs in a range of tempera-
ture that is characteristic of the starch source and the amount of
water [13]. This phase transition is associated with the diffusion of
water into the granule; as a result, there is a loss of optical birefrin-
gence and total loss of crystalline order. According to Hoover et al.
[14] there exists an amylose leaching as well as the apparition of a
new phase water-amylose/amylopectin.
Pasting: occurs after of gelatinization process and implicates
the granular swelling, exudation of the granular molecular com-
ponents, and eventually, total disruption of the granules; finalizing
is the formation of gel.
Retrogradation: is a process which describes the molecular
interactions between glucan molecules (by means hydrogen bond-
ing) in the gelatinized starch, after cooling. It also involves that
amylose and amylopectin form an ordered double-helical struc-
ture. These interactions occur after long time and low temperature.
Amylose is responsible for the short-term retrogradation [15].
Fig. 3 shows the conventional parameters used in the analysis
of a corn starch pasting profile (Sigma Aldrich, USA. CAS Number:
9005-25-8), in this case:
Pasting temperature: provides an indication of the minimum
temperature required to cook a given sample [16].
Peak viscosity: indicates the capacity and ability of water
“absorption of the starch granules”, and it is characterized by a
cessation of the swelling. At this point, an equilibrium take place
(4)
Breakdown:considered a measure of the disintegration degree
caused by the shear force of the starch granule or the paste stability
[18].
Setback: measure of the retrograde tendency during cooling
[19], and the increases in final viscosity due to the re-association
(cross-links) between starch chains (molecules) leached together
allowing formation of additional junction zones [5,9,20].
(5)
5. Results and discussion
5.1. Pasting profile
The changes in the pasting profile of the sample are governed
by the physical (morphology, gelatinization) and structural (inter-
action between macromolecules and the solvent) transformations
promoted by the heat and the “rotation” of the sample during the
experiment.
5.1.1. Morphological changes during a pasting profile
The changes in the morphology were studied in detail for Region
I, II, and III using SEM images taken at 1500× and 3500×. For Region
I, Fig. 4(A) and (B) shows the SEM images of corn starch gran-
ules for Point 1 taken at 66.12 ◦ C. At this temperature, the starch
granules retain the polyhedral morphology. Some granules exhibit
the presence of micro holes; however, all granules remain sepa-
rated. By direct inspection of Fig. 1(C), this point is located at the
beginning of the thermal transition identified as To . For Point 2
(Fig. 4(C) and (D)) taken at 74.81 ◦ C, the existence of branches that
interconnect granules is observed. These branches are formed by
some exuded amylose and amylopectin.This point is found after the
gelatinization temperature (see Fig. 1(C)), and SEM images show a
morphological change in the starch granules; however,the appar-
ent viscosity does not exhibit significant changes. An important fact
is that during the swelling of the starch granules and for the deter-
mination of the gelatinization temperature, the pasting profile is
not sensitive.
For point 3 (Fig. 4(E) and (F)) taken at 76.70 ◦ C is noticeable that
at this temperature the starch granules do not retain the original
shape, but that “donut” structures appear as a result of the heating
and shear rate of the starch granules. These “donuts” are inter-
connected between each other, which causes the system flow to
be lower in comparison with a particle suspension, producing an
increment in the apparent viscosity.
The starch gelatinization process took place between point 1 and
3 (see arrows in Fig. 2(A)). It is very important to note that the starch
granule (micro particles), under this condition, does not retain its
original shape, and it also means that starch as a microstructure
is not present in this part of the pasting profile, and that amylose
and amylopectin are outside of the original granules. Point 3, corre-
sponds to the peak of the first derivative of the pasting profile (see
Fig. 2(B)).
It is critical to point out that, according to the SEM images
correlated to the strong changes in the morphology of the sam-
ple is related to the starch morphology changes from granules to
“donuts”.
Point 4: the “donuts” break down now forming flakes as seen in
Fig. 4(G) and (H). This point corresponds to the peak viscosity for the
corn starch pasting. A more detailed inspection of this morphology
is presented in Fig. 4 H taken at 3500× which shows the formation
of a filamentous network (submicron) which interconnects these
flakes. These filaments cause the increase in the apparent viscos-
ity, which is governed by the exuded amylose and amylopectin and
by the formation of the filamentous network. It is very important
 N. Rincón-Londoño et al. / International Journal of Biological Macromolecules 91 (2016) 106–114 111

Fig. 5. SEM images of the morphological changes for region II (Points 5 and 6) and Region III (points 7–9) for pasting profile of isolated corn starch.

to note that for the peak viscosity, there are no starch granules
present. This result is not in agreement with that reported in the
RVA handbook [21], in which he reported that half of the starch
granules remained intact. According to Singh et al. [22] peak vis-
cosity is the point where the starch granules present the maximum
swelling. This result in the case of corn starch does not agree with
their results, because as it is shown in Fig. 4 (G) and (H) when
the water-starch suspension reaches the peak viscosity there are
not integer grains of starch which implied that the peak viscosity
cannot be related to the swelling power of the starch granules.
For region I, it is evident that the gelatinization process took
place in this temperature range and that the pasting properties are
governed not only by thermal changes, but also by the morphologi-
cal changes of the starch granules which plays a very important role
in the pasting profile. For this region the initial system is a starch-
water suspension, passed into a system with some integer starch
granules that are interconnected by biopolymers; then the system
is transformed by “like-donuts” connected between them, and due
to the rotation and the change in the temperature, the morphol-
ogy of the system passes a flakes interconnected network (peak
viscosity).
For region II (Fig. 5(A) to (D), isothermal region), a decrease of
the apparent viscosity (point 5 and 6) is evident. The drop in the
apparent viscosity is due to the disintegration of the starch gran-
ules at a high temperature, but by direct inspection of Fig. 4(A) to
(F) the disintegration of the starch granules occurs during the gela-
112 N. Rincón-Londoño et al. / International Journal of Biological Macromolecules 91 (2016) 106–114
Fig. 6. Structural changes of the dry freezing samples obtained for each one of the points selected in the pasting profile of isolated corn starch.
tinization process. Our explanation for the drop of the apparent
viscosity is based on the changes of the morphology: the system
goes from an interconnected filamentous network to an intercon-
nected flakes layer. These flakes become aligned with the parallel
layers (hydrogel), and this phenomenon in the isothermal region
produces a decrease in the apparent viscosity. SEM studies in this
region reveal that in the so called breakdown (point 6) a total align-
ment of the flakes occurs giving as a result the reduction of the shear
stress and decreases in the apparent viscosity.
For region III (points 7–9, cooling process), the sample remains
with the same flakes morphology shown in Fig. 5(E)–(J). The
increase in the apparent viscosity can be related to the reduction of
the total internal energy of the system (decrease of temperature)
and the increases of the shear stress between the layers formed by
flakes.
5.1.2. Structural changes
The morphological changes of sample as a result of the temper-
ature can be related to the changes in the starch structures. Fig. 6
shows the X-ray diffraction patterns of the freezing samples taken
for each one of the points described in Fig. 2(A). Point 1, which is
located at the beginning of the endothermic peak (see Fig. 1(C)),
the starch is integer (see Fig. 4(A) and (B)) and the sample exhibits
a semi crystalline structure, indicating that no gelatinization took
place even the temperature increases and water becomes to dif-
fuse into the starch grains (Fig. 6(A)). For point 2, (See Fig. 4(C)
and (D)) the pattern (beginning of the gel formation) still showed a
remaining crystallinity, indicating that this sample is still undergo-
ing the gelatinization process, and that this point is located inside
of the endothermic peak. By detail inspection of the points 3–9, it is
evident that the X-ray diffraction patterns show an amorphous sys-
tem. The SEM images and X-ray diffraction patterns are conclusive,
indicating that the crystalline order of amylose and amylopectin
macromolecules occurs exclusively inside of the micro particle
called starch.
5.1.3. Thermal changes
In order to understand the correlation between thermal changes
that occurs during pasting profiles, the thermograms of freeze dried
samples were studied using DSC. Fig. 7(A) to (I) show the charac-
teristic of thermograms for each one of these points. For point 1, it
is characterized by an endothermic transition, which implies that
the amylose and amylopectin inside starch granules at this point
still have the internal order. This result is confirmed by the X-ray
diffraction pattern shown in Fig. 6(A) in which a clear semi crys-
talline structure is present and correlated to the SEM images shown
in Fig. 4(A) and (B). The thermogram for point 2 showed a remain-
ing endothermic peak, which is indicative of some crystalline order
inside of the starch granules that can be corroborated by the anal-
ysis of the X-ray diffraction pattern shown in Fig. 6(B), and by the
existence of starch granules shown in Fig. 4(C) and (D). For points
3–9 (hydrogel system) in the case of corn starch, no crystalline
structures were found, even for points 8 and 9. This result is very
important in terms of the pasting interpretation because accord-
 N. Rincón-Londoño et al. / International Journal of Biological Macromolecules 91 (2016) 106–114
Fig. 7. Thermal profiles of dry freezing samples obtained for each one of the points selected in the pasting profile of isolated corn starch.
ing to the SEM images, X-ray patterns, and DSC thermograms, no
recovery of the crystalline order is evident. Taking into account the
amorphous patterns for points 8 and 9, no molecular reorganiza-
tion took place in this region (setback), and SEM, DSC, and X-ray
diffraction showed that no retrogradation. This means that during
a pasting profile the retrogradation does not take place and some
misinterpretation in the literature are often reported.
5.2. Analysis about of the phenomena occurred during a pasting
profile
The changes in the pasting profile for isolated corn starch are
influenced by different physicochemical changes that take place as
result of the temperature, water, and constant shear rate applied
during the test. Taking into account the X-ray diffraction, DSC, and
SEM images results, during the pasting profile for isolated corn
starch, some phenomena that take place during a pasting profile
of corn-starch can be analyzed as follows:
Pasting: network formation of a gel and occurs after of gela-
tinization process. Taking into account Fig. 1(C) where To and Te
are shown, in this range of temperature the gelatinization of starch
occurs. We can conclude that the pasting profile is not able to deter-
mine the range of temperature in which the gelatinization occurs.
DSC is a better tool to determine the beginning and end of the
gelatinization.
Pasting temperature: defined as a range of temperature after the
gelatinization of starch in which the system undergoes new hydro-
113
gel morphology, it can be defined by the use of the first derivative
of the pasting profile (peak maximum) and begins at the end of the
gelatinization (Te ), and finished when the hydrogel is formed.
Peak viscosity: indicates the end for the stable hydrogel forma-
tion with characteristic morphology (interconnected micro fibrils).
SEM images shown in Fig. 4(G) and (H) confirm this event. On the
other hand, the temperature at peak viscosity can be defined as the
temperature in which the gel finalizes the formation, and at this
point no starch granules are integer.
Breakdown: the decrease in the apparent viscosity for the
isothermal region of the pasting profile at constant rotation (rpm) is
independent of the temperature and it is originated by the reduc-
tion of the internal shear stress between the layers formed due
to rotation of the sample. In the case of corn starch, the planes
are formed by flakes. Breakdown can therefore be understood as
the minimum value of the apparent viscosity of the sample at the
end of the isothermal region of the pasting profile. According to
our analysis, it is not caused by the disintegration of the starch
structure caused by the shear forces [18], because at this time and
temperature the system is already a hydrogel.
Setback is originated by the reduction of the temperature of
the system and it is related to the changes in the internal shear
stress between planes. According to our results, it does not have
any relationship with retrogradation, because as can be seen in the
detailed study of the structural changes shown in Fig. 6(I) (Point
9 for the pasting profile of corn starch) for the end of the past-
ing profile of isolated corn starch, no recrystallization took place
114 N. Rincón-Londoño et al. / International Journal of Biological Macromolecules 91 (2016) 106–114
due to the cooling process. It is clear that in the case of the micro
flakes formed during the pasting profile of corn starch-water sus-
pension, the reduction in the temperature originated the increases
in the apparent viscosity, increase the shear stress between them.
The retrogradation occurs after gelatinization and it is defined as
the transition from an amorphous state to a crystalline state (more
orderly). The changes that occur during phenomenon can be moni-
tored by X-ray Diffraction [23]. This instrumental technique is used
for determinate and identified the long atomic order of a sample.
On the other hand, the studies performed on retrogradation report
a time of storage of the sample and this condition is not comply in
the work. It has been reported the evident of retrogradation in sam-
ples storage by 14 days used DSC from 20 to 120 ◦ C, the transition
peak is observed [24]. Therefore, we consider that the final viscos-
ity is not a parameter indicating the retrogradation of the starch
compounds and this was corroborated by X-ray Diffraction.
6. Conclusion
Changes in the viscosity profile of corn starch are influenced
by different physicochemical changes taking place as a result of
temperature, and shearing force applied during the measurement
due to the constant rotation of the starch-water suspension and
after gelatinization the hydrogel. Considering the morphological
changes of the starch water suspension along the pasting pro-
file, these changes governed the behavior of the curve of viscosity
profile. Moreover, during the viscosity profile structural and ther-
mal changes in starch were observed, which ends after that the
starch gelatinization occurred. X-ray Diffraction studies confirm
that during the cooling process of the hydrogel, no retrogradation
was observed. An important point in the case of the study of past-
ing profiles of starch is that is necessary to determine the region.
Dilute, transition, and concentrate, in which these experiments can
be obtained, then is necessary to run experiments with different
starch/water ratios.
Acknowledgements
This work was partially supported by Conacyt (Consejo Nacional
de Ciencia y Tecnologia) (National agreement studentship, No.
293329). We thank Carmen Peza, M. en I.Q. Alicia del Real López,
and Dr. Beatriz Millan (CFATA-UNAM) for their technical support.
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