International Journal of Biological Macromolecules 183 (2021) 1723–1731

Contents lists available at ScienceDirect

International Journal of Biological Macromolecules

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

Study of morphological, structural, thermal, and pasting properties of

flour and isolated starch from unripe plantain (Musa paradisiaca)
Lineth J. Vega-Rojas a, Sandra M. Londoño-Restrepo b, Mario E. Rodriguez-García b,⁎
a
Laboratorio de Biología Celular y Molecular, Facultad de Ciencias Naturales, Universidad Autónoma de Querétaro, Av. de las Ciencias s/n, Juriquilla, Querétaro 76230, Querétaro, Mexico
b
Departamento de Nanotecnología, Centro de Física Aplica y Tecnología Avanzada, Universidad Nacional Autónoma de México, Querétaro, Qro. 76230, Mexico

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

Article history: This work focused on studying the mineral composition, morphology, thermal, structural, and pasting properties
Received 8 April 2021 of isolated plantain starch. Plantain starch is rich in K, and other ions as Mg, Ca, P, and Si were found. This starch
Received in revised form 18 May 2021 exhibits lenticular, elliptical, and semispherical morphologies. Two endothermal events present in the thermo-
Accepted 20 May 2021Available online 27 May
gram were identified as the hexagonal and orthorhombic solvation. C-type starch formed by hexagonal and or-
2021
thorhombic nanocrystal was completely indexed. The ash content showed the presence of calcium phosphate
Keywords:
(KCaP2O7), Calcium Magnesium Phosphate (Ca2.71Mg0.29(PO4)2), and silicon oxide (SiO2). The pasting profile of
Plantain this starch behaves between a custard and a hydrogel. Scanning electron microscopy of the lyophilized samples
Starch along pasting profile confirms that the shear and van der Walls forces and slurry morphology govern the pasting
C-type starch profile changes.
Orthorhombic structure © 2021 Published by Elsevier B.V.
Hexagonal structure

1. Introduction
Plantain is native of South East Asia, belongs to the genus Musa of the
family Musaceae. In the last centuries, it was spread worldwide, partic-
ularly in the equatorial region that satisfies sun requirements and hu-
midity for its good development. Plantain has been incorporated in
human and animal diets from Mexico to Peru, and unripe and ripe plan-
tain is consumed equally in soups, chips, cake, mash, among others [1].
Plantain is considered a basic fruit in food due to its production all year
and flavor; it can be processed as flour or isolated starch for human
consumption.
Starch is an essential fraction of the different products. Its content in
cereals (corn, wheat, rice) varies from 30 to 80%, in legumes (bean, peas,
lentil) from 25 to 50%, in tubercles (potato, yucca) from 60 to 90%, and
in some fruits (banana and mango) is around 70% in the dry base [2].
It is expected that the physicochemical properties of starches from the
same botanical sources exhibited similar behavior. Aspects related to
chemical and mineral composition still are an open research problem.
Plantain flours are used to develop edible films to reduce the use of
petroleum-derived polymers. Gutiérrez and González [3] produced ed-
ible films based on plantain starch added with Aloe vera natural fibers
using the casting method. They found that these films exhibited
smoother, more transparent, more rigid and plastics, less moist, and
more hydrophobic surfaces. This application of plantain starch opens a
new window of opportunities for several applications of starches.
⁎ Corresponding author.
E-mail address: marioga@fata.unam.mx (M.E. Rodriguez-García).
Even though many studies about the isolated plantain starches char-
acterization, some aspects related to the crystalline structure and ther-
mal and pasting properties are still an open problem, and their
elucidation could contribute to their future application. One of these ex-
amples is the complete X-ray indexing of the isolated starches from
musaceous. Of course, these properties depend on agronomical and en-
vironmental conditions. Rodriguez-García et al. [4] pointed out that the
so-called A-type starch possesses orthorhombic nanocrystals and B-
type hexagonal ones. Meanwhile, C-type does not correspond to a
new crystalline structure. From a crystallographic point of view, this
starch has orthorhombic and hexagonal crystals.
Concerning the pasting properties, most of the published articles es-
tablish as a rule starch/water ratio to be 3/18. However, according to
Acosta-Osorio et al. [5] and Gutiérrez-Cortez et al. [6], for the proper in-
terpretation of any pasting profile, this must be carried out in the tran-
sition regimen. It is necessary to determine for any sample the starch/
water ratio that satisfies this regimen. It is characterized by no signifi-
cant changes in the peak viscosity as a function of the starch/water
ratio. Intrinsic parameters such as the grain size, chemical and mineral
composition, crystalline structure, and amylose/amylopectin ratio; and
extrinsic parameters such as extraction, particle size, moisture, among
others govern a pasting profile.
Zobel et al. [7] defined gelatinization as the melting of crystallites in
starch; however, there was no specification about what kind of crystals
contribute to the melting. Starch gelatinization is related to the water
solvation of orthorhombic and hexagonal crystals. In the case of C-
type starches, in which both crystalline structures are present, the gela-
tinization should include the thermal transition for each one of them. So

https://doi.org/10.1016/j.ijbiomac.2021.05.144
0141-8130/© 2021 Published by Elsevier B.V.
L.J. Vega-Rojas, S.M. Londoño-Restrepo and M.E. Rodriguez-García
far, the lack of knowledge of the crystalline structures in starch defines
gelatinization as an order-disorder transition. Still, it is most related to
the solvation process.
Pelissari et al. [8] studied the chemical, physical, structural, morpho-
logical, and pasting properties of banana flour and starch. However, the
flour and starch extraction was through potassium metabisulfite solu-
tion, generating changes in the structure, morphological, chemical,
and pasting properties.
This research aims to study the elemental composition, chemical,
morphological, and structural properties of plantain flour and starch
and analyze the pasting profile of isolates plantain starch as a function
of the time by using scanning electron microscopy images, and the cor-
relation between these properties.
2. Material and methods
2.1. Plantain flour preparation
Dominico Harton plantains harvested after eight weeks of flowering
in Armenia, department of Quindio, Colombia, at an altitude of
1551 masl, an average temperature of 22.5 °C, and 76% relative humid-
ity, according to the methodology proposed by [1]. After pealing, they
were cut in slices 1 mm thick and submerged in cool water (4 °C) for
1 h to avoid oxidation and fermentation, and to avoid the use of potas-
sium metasulfide solution. The central part of the slices was removed
and mixed in a blender (kurp-Germany) for 3 min, and then centrifuged
for 20 min to 2800 rpm. Finally, the precipitate was dried at 40 °C for
12 h. Fig. 1A shows unripe plantains, and Fig. 1B exhibits dried slices
of plantain before removing of their central part.
2.2. Starch preparation
Plantain isolated starch was obtained using the methodology used
by [9]. In brief: unripe plantains were peeled and cut into slices, and
its central part removed. 100 g of the sample was macerated with
200 g of cool distilled water at 4 °C using a Kurp blender for 3 min.
The slurry was kept at 4 °C until precipitation and then was centrifuged
for 20 min at 2800 rpm. The sample was washed three times with dis-
tilled water. Finally, the starch was dried in a furnace (40 °C, for 8 h).
2.3. Chemical proximate analysis
Moisture content of the plantain flour was determined using
Method 925.10 and Method 920.86 for crude fiber content [10]. Ash,
protein, and fat content were measured by using Approved Methods
08-01, 46-13, and 30-25 [11], respectively. All the measurements were
made in triplicate.
Fig. 1. (A) Unripe Dominico Harton plantains. (B) Transversal slices of plantain.
1724
International Journal of Biological Macromolecules 183 (2021) 1723–1731
2.4. Amylose content
Total starch and amylose content were determined for plantain
starch using the Megazyme assays K-TSTA and K-AMYL kits, respec-
tively. Total starch quantification is based on enzymatic hydrolysis
with amylase and amyloglucosidase to produce glucose, while amylose
determination involves precipitating it with Concanavalin-A [1].
2.5. Mineral content by ICP-OES
The mineral content in isolated plantain starch was determined
using an Inductively Coupled Plasma optical emission spectrometer
(ICP- OES, model Thermo iCAP 6500 Duo View). Then, 0.1 g of the starch
was digested with nitric acid (Baker 69–70%) and it was made in tripli-
cate. Upon return to the ground state, the elements excited by the argon
plasma were then identified by their characteristic emission spectra.
Emission intensity was then converted to elemental concentration by
comparing to a standard curve.
2.6. Sample characterization by LV-SEM
Plantain, plantain flour, and isolated starch, as well as the samples
obtained from the pasting profile, were performed in a low-vacuum
Scanning electron microscope (LV-SEM), JSM 5600LV, with a resolution
of 5 nm in LV mode. The analysis was performed using equipment con-
ditions of 20 kV electron acceleration voltage and 12–20 Pa of pressure
in the specimen chamber, obtaining the images on the fracture surfaces
with the backscattering electron signal.
2.7. X-ray diffraction characterization
X-ray diffraction patterns of isolated plantain starch and ash from
flours were obtained on a diffractometer (Rigaku, ultima IV) with a de-
tector D/tex ultra, operating at 35 kV and 15 mA, with a CuKα radiation
wavelength of 0.15406 nm, and from 5 to 70° on a 2θ scale with a step
size of 0.02°.
2.8. Differential scanning calorimetry (DSC)
The DSC thermogram of the starch was measured using a Differential
Scanning Calorimeter DSC 1 (Mettle Toledo, Greifensee-Switzerland) and
data was processed with TA Instrument software. Calibrations were per-
formed using pure indium. Samples of 12.0 ± 0.1 mg were prepared by
adding deionized water to the samples into the pan until they reach a
moisture of 85% (w/w). The aluminum pans were hermetically sealed
and kept at room temperature for 6 h. The samples were scanned from
30 to 110 °C at 7.5 °C/min. Each experiment was conducted in triplicates.
L.J. Vega-Rojas, S.M. Londoño-Restrepo and M.E. Rodriguez-García
2.9. Measurement of the pasting profile
The apparent viscosity of isolated starch was determined using a
rheometer (Anton Paar MCR-102; United Kingdom) with 3 g of starch
and 18 mL of water (85.7% moisture). The following thermal profile
was used: Initially, the temperature of the system was 50 °C, and it
remained constant for 1 min. Then, the sample was heated for 5.3 min
from 50 to 90 °C; next, it was held at a constant temperature of 90 °C
for 5.3 min (isothermal condition); after that, the sample was cooled
down to 50 °C for 5.3 min, and finally, this temperature was kept con-
stant for 1 min. The frequency of the system was set to 193 rpm.
Following the methodology proposed by [6], four point along the
viscosity curve were chosen to be analyzed in detail: (1) during gelati-
nization, (2) peak viscosity, (3) breakdown, and (4) end viscosity.
When the system reached each point, the rheometer was immediately
stopped, and the sample is cooled in liquid nitrogen and freeze-dried
using a freeze dry Freezone 2.5 (Labconco, Kansas City, USA), for 48 h.
3. Results
3.1. Chemical proximate analysis
Table 1 shows the content of moisture, ash, fat, crude fiber, and pro-
tein for plantain flour and starch. The ash content reduction is origi-
nated from the removal of some minerals from the fat and protein.
The isolation method used in this work reduces the fat and protein con-
tent that could be associated with the removal of insoluble and soluble
fiber fractions. Mutis-Gonzalez et al. [12] reported 10.13% moisture,
0.33% ash, 0.15% fat, 0.18% fiber, and 1.75% protein for unripe
Dominico-Harton plantain starch. These values indicate that the isola-
tion process followed in this work achieved a more efficient extraction.
3.2. Total starch and amylose content
Total starch for the isolated starch was 91% which means the isola-
tion process is highly effective. According to Table 1, the remainder per-
centage corresponds mainly to absorbed water and small amounts of
protein, fiber, ash, and fat. Meanwhile, amylose represents 16% of the
starch, which is in accordance with Quintero-Castaño et al. [1] that re-
ported 14% amylose for Dominico hartón plantain. This finding means
that plantain is a source of amylopectin-rich starch.
3.3. Mineral content
Fig. 2 presents the quantification of the trace minerals present in the
starch. Isolated plantain starch is rich in K, this ion influences other
physicochemical properties as pasting profile. Mutis-González et al.
[12] explored the effect of adding K and Mg to plantain starch on its
thermal, pasting, and functional properties. Both ions trend towards vis-
cosity recovery because of the re-ordering of the polymeric chains. Their
presence also conducted to an increase in the gelatinization tempera-
ture compared to the control sample. These authors suggested that
Mg becomes part of the structure since an infrared band is modified
after adding to the starch.
3.4. Plantain flour and starch characterization by LV-SEM
Fig. 3A and B shows SEM images of a transversal cut of unripe plan-
tain (see Fig. 1B) taken at 500× and 1000×, respectively. Starch granules
Table 1
Chemical proximate values for plantain flour and starch.
Sample Moisture (%) Ash (%) Fat (%) Crude fiber (%) Protein (%)
Flour 6.91 ± 0.18 1.23 ± 0.12 2.007 ± 0.341 0.039 ± 0.001 13.13 ± 0.25
Starch 7.53 ± 0.95 0.08 ± 0.05 0.015 ± 0.091 0.038 ± 0.002 1.30 ± 0.10
1725
International Journal of Biological Macromolecules 183 (2021) 1723–1731
Fig. 2. Mineral content by ICP-OES of unripe plantain starch.
are in hexagonal bags of fiber with about 50 μm width. Fig. 3B shows
membranes covering the starch granules, which corresponds to soluble
fiber (gums, mucilage, and pectin). Fractions of the insoluble fiber
(cellulose, hemicellulose, and lignin) are also presented (see blue cir-
cles). Fig. 3C and D corresponds to the SEM images of the flour in
which disaggregate granules and cumuli are present. Soluble and insol-
uble fibers have been fractioned due to the milling process. Fig. 3E and F
exhibits the isolated starch, in which (a) lenticular, (b) elliptical, and
(c) semispherical morphologies are present. Lenticular granules have
a diameter from 10 to 15 μm; elliptical, between 15 and 32 μm length
and 0 to 15 μm width; semispherical ones have a diameter ranging
from 8 to 12 μm. As can be seen, the methodology used to obtain iso-
lated starch produce starch without fiber.
3.5. X-ray analysis
Fig. 4A shows the high-resolution X-ray diffraction (XRD) pattern of
the isolated plantain starch. Black dash lines correspond to the ortho-
rhombic structure indexing, while red ones to hexagonal crystalline
structures reported by Rodriguez- Garcia et al. [4], being predominant
the hexagonal phase. Table 2 exhibits the position of the peaks using
the second derivative criteria, the Miller indexes for each one of the
diffracted peaks and their respective crystalline phase.
The orthorhombic structure is present in A-types starches such as
amaranth [6] and sorghum [13]. Hexagonal structure is present in B-
type starches. When both structures are in any starch, this is classified
as C-type; usually found in starches from legumes [14]. Exceptions to
this classification based on the source have been nonetheless reported,
as was the case of avocado pit starch [4]. The isolated plantain starch ex-
hibits simultaneously orthorhombic and hexagonal pyro glucan struc-
tures, namely, a C-type starch. It means that this C-type starch pattern
is nothing, but a convolution of the diffraction peaks produced by both
orthorhombic and hexagonal structures. Recently, Guo et al. [15] re-
ported A-, B- and C-type starch granules coexist in the root tuber of
sweet potato. However, this is a misinterpretation since, so far only
two crystalline structures have been found in starches. Soares et al.
[16] classified plantain starch as C-type, but they did not show its
indexation.
Peak broadening is originated from the nanometric size of the crys-
tal, as was reported by [17,18]. The presence of both crystalline struc-
tures influences its thermal and pasting physicochemical properties.
Fig. 4B displays the XRD pattern of the ash obtained by calcination of
the flour identifying: potassium calcium phosphate (KCaP2O7), Calcium
Magnesium Phosphate (Ca2.71Mg0.29(PO4)2), and silicon oxide (SiO2).
For their identification ICDD (International Center for Diffraction Data)
L.J. Vega-Rojas, S.M. Londoño-Restrepo and M.E. Rodriguez-García
Fig. 3. (A) and (B) Transversal cut of unripe plantain. (C) and (D) plantain flour. (E) and (F) plantain starch. Images were recorded at 500× and 1000×, respectively.
cards 00–050-1563, 04–010-2972, and 01–077-8628 were used, re-
spectively. The presence of these compounds agrees with ICP-OES find-
ings in which K, P, Ca, Mg, and Si were found. Plantain ash has been used
to enhance mineral absorption by animals [19], and its consumption im-
proves the mineral intake in human diets.
3.6. Differential scanning calorimetry analysis
Gelatinization is defined as an order-disorder transition of the crys-
talline components in starch. Fig. 5A shows the thermogram for the
1726
International Journal of Biological Macromolecules 183 (2021) 1723–1731
starch in which onset (T1o), peak (T1p), and end (T1e) temperatures
are indicated. However, a second endothermal transition is observed
by simple inspection, and its range identified using the second deriva-
tive criteria (Fig. 5B). This phenomenon obeys the presence of ortho-
rhombic and hexagonal crystalline structures of pyro glucans, as
shown in Fig. 4A. When they are in contact with water and heat, they
solvate and produce two T1p and T2p. T1p transition could be associated
with the solvation of hexagonal structures while T2p with orthorhombic
ones. This assumption is based on two facts: first, the number of water
molecules in the hexagonal structures is bigger than in the orthorhombic
L.J. Vega-Rojas, S.M. Londoño-Restrepo and M.E. Rodriguez-García International Journal of Biological Macromolecules 183 (2021) 1723–1731

Fig. 4. (A) X-ray diffraction pattern of isolated unripe plantain starch. (B) X-ray diffraction
pattern of the ash obtained from plantain flour. Fig. 5. (A) DSC thermogram of isolated plantain starch and (B) its second derivative.

one [4,20,21]. Secondly, the XRD pattern exhibits a predominant hexag- not explain the reason of the differences in the gelatinization tempera-
onal structure, and T1p is the most predominant thermal event. Guo et al. ture for these structures. The isolation process produced starch with
[15] found using DSC that the A-, B- and C-type starch granules have sig- low-fat content, and then the so-called amylose-lipid complex is not
nificantly different gelatinization initial and end temperatures. However, present.
they did not index the hexagonal and orthorhombic structures, and did
3.7. Pasting profile
Table 2
Peak position, Miller indexes and crystal structures present in isolated unripe plantain 3.7.1. Determination of the pasting regimen
starch [4]. The rheological problem to determine the apparent viscosity has
Peak position (°) Miller indexes Crystalline phase been studied in detail [22,23]. This author considered the existence of
5.72 (010) Hexagonal
inter-particle force within the concentrate suspension. The forces can
8.91 (100) Orthorhombic form aggregates or cumuli, which are responsible for significant viscos-
10.17 (011) Hexagonal ity changes. Quemada's model showed that the increase in the effective
11.28 (101) Orthorhombic volume fraction of particles in the suspension increases the apparent
14.15 (021) Hexagonal
viscosity. On the other hand, Gutiérrez-Cortez et al. [6] showed that
15.22 (200) Orthorhombic
17.25 (121) Hexagonal the increase in the apparent viscosity before peak viscosity is due to
(031) Orthorhombic the exudation of amylose and amylopectin forming a disordered matrix.
18.22 (220) Orthorhombic Fig. 6A shows pasting profiles for seven different starch/water ratio:
20.12 (040) Orthorhombic 1.5/19.5, 2/19, 2.5/18.5, 3/18, 3.3/17.7, 3.5/17.5, and 3.6/17.4. As can be
22.29 (131) Hexagonal
23.03 (231) Orthorhombic
seen, small variations in the water produce strong changes in the past-
24.21 (032) Hexagonal ing profile. All these starch/water suspensions were done to determine
26.45 (013) Hexagonal the best rheological condition to obtain a pasting profile within the tran-
30.55 (060) Orthorhombic sition regimen considering the peak viscosity as a criterion [6]. Fig. 6B
31.46 (142) Hexagonal
shows the behavior of the peak viscosity versus starch/water ratio. In
32.93 (233) Orthorhombic
33.26 (143) Orthorhombic plantain starch, the 3/18 ratio proved to be the best rheological condi-
34.56 (060) Hexagonal tion for the apparent viscosity analysis.
38.36 (161) Hexagonal The curve for the 3/18 (starch/water) ratio showed in Fig. 6C was di-
43.78 (442) Hexagonal vided into four different time windows to analyze the changes in the
47.11 (424) Orthorhombic
pasting profile. The window I (0 to 280 s; 70.23 °C), in which no changes

1727
L.J. Vega-Rojas, S.M. Londoño-Restrepo and M.E. Rodriguez-García
Fig. 6. (A) pasting profile for seven starch/water ratio mixtures: 1.5/19.5, 2/19, 2.5/18.5, 3/18, 3.3/17.7, 3.5/17.5, and 3.6/17.4. (B) Diluted, transition, and saturated regimens based on peak
viscosity behavior as a function of the starch/water ratio. (C) Viscosity profile for the 3/18 ratio mixture stopped at four different points along the curve.
in the apparent viscosity values as a function of the increase of
temperature and time were apparently not observed. However, using
the second derivative criteria, the pasting temperature is 68.41 °C
(260 s) which is between the gelatinization range. It means that it is
possible to obtain information about gelatinization from the pasting
profile. Currently, according to Fig. 5, the gelatinization is taking place
at T1o = 65.36 °C (228 s), ending at T1e = 71.80 °C (296 s). These results
indicate that the first increase of the viscosity is related to the gelatini-
zation. This fact could indicate that starch granules are collapsed, but
not necessarily disrupted. Our onset temperature agrees with the values
reported by Dufour et al. [24], Chávez-Salazar et al. [25] and Montoya
et al. [26]. Discrepancies in the reported values are directly related
with the used starch/water ratio.
According to Zobel et al. [7], gelatinization is directly related to the
ordered to disordered structural transition. However, they did not spec-
ify what kind of crystalline structure. Recently, Gutiérrez-Cortez et al.
[6] showed that gelatinization is directly related to crystal solvation.
The isolated plantain starch is composed mainly of hexagonal crystals,
but the orthorhombic structure is simultaneously present.
Window II (280 to 444 s; 85.67 °C) exhibits the heating region that
ends with the maximum develop of viscosity (14,186 cP) whose ease
of cooking was 444 s or 7.4 min. In this region, an abrupt change in
the pasting profile take place. According to the DSC thermogram, the
end of gelatinization took place. In this window, all granules are broken,
amylose and amylopectin chains exuded and disrupted. And more
important, hexagonal and orthorhombic crystals are solvated, releasing
glucopyranosyl units. The increase is related to the disordered slurry
originating strong torque in the system to maintain 193 rpm.
Oseguera-Toledo et al. [27] showed in malted barley that even solvation
1728
International Journal of Biological Macromolecules 183 (2021) 1723–1731
of the orthorhombic nanocrystals, glucopyranosyl units does not con-
tribute to the increases in the apparent viscosity.
Window III (444 to 802 s; 92 °C) corresponds to the breakdown
(10,075 cP) of the pasting profile during the holding. A decrease in the
apparent viscosity could be produced by the slurry organization having
a reduction in the sheer force and maybe due to the formation of
microchannel forming a hydrogel as was proved by [28,29].
Window IV (802 to 1380s; 49.94 °C) corresponds to the total setback
region (5007 cP) during the cooling process and final holding that ends
with the final viscosity (9113 cP). The shear and Van der Walls forces in-
creases, and the molecular reordering of amylose and amylopectin
could take place originating a relative increase in the apparent viscosity.
This reordering does not produce recrystallization or retrogradation.
According to Cornejo-Villegas et al. [30], the slurry behaves as a custard
when the end viscosity increases, but as a hydrogel when the end vis-
cosity is lower that the peak viscosity. A custard does not have kine-
matic viscosity. In the case of plantain starch, this behavior is between
a custard and a hydrogel.
3.7.2. Morphological changes during the development of the viscosity
profile
To analyze the pasting profile behaviors, each sample was cooled and
lyophilized at the end of each time window and analyzed using SEM im-
ages, following the methodology proposed by [6]. Fig. 7 shows the four
studied windows along the pasting profile taken at 500× and 2500 ×.
Fig. 7A and B shows that de starch granules collapsed, but most of
them are still integer, indicating that gelatinization took place and the
internal order of the starch grain was disrupted. At this point, it is pos-
sibly that the amylose and amylopectin molecules absorb water and
L.J. Vega-Rojas, S.M. Londoño-Restrepo and M.E. Rodriguez-García International Journal of Biological Macromolecules 183 (2021) 1723–1731

Fig. 7. SEM images of the lyophilized samples at the end of each time window along the pasting profile.

1729
L.J. Vega-Rojas, S.M. Londoño-Restrepo and M.E. Rodriguez-García
the mixture and begin to swell. SEM images showed in Fig. 7C and D
corresponds to the maximum viscosity. The formation of disordered
flakes-like clusters formed by exuded amylose and amylopectin mole-
cules explain the abrupt increase in the apparent viscosity. Rincón-
Londoño et al. [28] also reported the formation of these flakes in
maize starch.
Fig. 7E and F shows the SEM images taken at the point denominated
break down, which corresponds to the end of the isothermal region.
This image shows that the slurry is ordered, and the micro holes allow
the water interconnected movement due to the rotation of the system.
These ordered holes explain the reduction of the apparent pasting
viscosity.
Fig. 7G and H shows the SEM image of the paste obtained at the end
of the pasting profile in which the micro-holes network is formed dur-
ing the cooling process. The micro-holes vary from 10 to 25 μm.
The role of the ions presents in the starch and in the paste is still an
open problem that requires a more detailed analysis. It has been found
that Ca++ in corn paste originates a decrease in the end viscosity, pro-
moting the gel formation [30].
4. Conclusions
This work shows that plantain starch is rich in K but contains other
ions such Ca, Mg, P, and Si. Isolated plantain starch exhibits lenticular,
elliptical, and semispherical morphologies. According to the complete
X-ray results, this starch exhibits hexagonal and orthorhombic nano-
crystalline structures and can be classified as C-type. The ash X-ray char-
acterization showed the presence of potassium calcium phosphate
(KCaP2O7), Calcium Magnesium Phosphate (Ca2.71Mg0.29(PO4)2), and
silicon oxide (SiO2). Solvation of the hexagonal and orthorhombic struc-
tures explains the existence of two endothermal events. The behavior of
the pasting properties was explained using SEM images and indicates
that the changes in the slurry morphology, and shear and van de
Walls forces govern it. The pasting profile behaviors indicate that this
starch can be used in infantile formulations due to its behavior between
a custard and a hydrogel. It does not present dynamic viscosity and
would not have problems when swallowed.
CRediT authorship contribution statement
Lineth J. Vega-Rojas: Investigation and Validation.
Sandra M. Londoño-Restrepo: Validation, Formal Analysis, Writing –
Original Draft, Writing - Review & Editing, and Visualization.
Mario E. Rodriguez-García: Conceptualization, Methodology,
Formal Analysis, Writing – Original Draft, Writing - Review & Editing,
and Supervision.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgments
This work was supported by Laboratorio Nacional de Caracterizacion
de Materiales-Conacyt at CFATA-UNAM. S. Londoño-Restrepo thanks
CFATA-UNAM for her postdoctoral position and CONACYT for the financial
support. J. Vega-Rojas thanks Conacyt for her postgraduate scholarship.
Authors thank Dr. Beatriz Millan -Malo for the X-ray technical support.
References
[1] V.D. Quintero-Castaño, F.J. Castellanos-Galeano, C.I. Álvarez-Barreto, J.C. Lucas-
Aguirre, L.A. Bello-Pérez, M.E. Rodríguez-Garcia, Starch from two unripe plantains
and esterified with octenyl succinic anhydride (OSA): partial characterization,
Food Chem. 315 (2020), 126241, https://doi.org/10.1016/j.foodchem.2020.126241.
1730
International Journal of Biological Macromolecules 183 (2021) 1723–1731
[2] E. Flores-Gorosquera, F.J. García-Suárez, E. Flores-Huicochea, M.C. Núñez-Santiago,
R.A. González-Soto, L.A. Bello-Pérez, Rendimiento del proceso de extracción de
almidón a partir de frutos de plátano (Musa paradisiaca). Estudio en planta piloto,
Acta Cient. Venez. 55 (1) (2004) 86–90.
[3] T.J. Gutiérrez, G. González, Effect of cross-linking with Aloe vera gel on surface and
physicochemical properties of edible films made from plantain flour, Food Biophys.
12 (1) (2017) 11–22, https://doi.org/10.1007/s11483-016-9458-z.
[4] M.E. Rodriguez-Garcia, M.A. Hernandez-Landaverde, J.M. Delgado, C.F. Ramirez-
Gutierrez, M. Ramirez-Cardona, B.M. Millan-Malo, S.M. Londoño-Restrepo, Crystal-
line structures of the main components of starch, Curr. Opin. Food Sci. 37 (2021)
107–111, https://doi.org/10.1016/j.cofs.2020.10.002.
[5] A.A. Acosta-Osorio, G. Herrera-Ruíz, P. Pineda-Gómez, M.A. Cornejo-Villegas, F.
Martínez-Bustos, M. Gaytán, M.E. Rodríguez-García, Analysis of the apparent viscos-
ity of starch in aqueous suspension within agitation and temperature by using rapid
visco analyzer system, Mech. Eng. Res. 1 (1) (2011) 110–121, https://doi.org/10.
5539/mer.v1n1p110.
[6] E. Gutiérrez-Cortez, E. Hernández-Becerra, S.M. Londoño-Restrepo, M.E. Rodriguez-
García, Physicochemical characterization of Amaranth starch insulated by mechan-
ical separations, Int. J. Biol. Macromol. 177 (2021) 430–436, https://doi.org/10.
1016/j.ijbiomac.2021.02.138.
[7] H.F. Zobel, S.N. Young, L.A. Rocca, Starch gelatinization: an X-ray diffraction study,
Cereal Chem. 65 (6) (1988) 443–446.
[8] M.F. Pelissari, M.A. Andrade-Mahecha, J.P. Amaral Sobral, C.F. Menegalli, Isolation
and characterization of the flour and starch of plantain bananas (Musa paradisiaca),
Starch-Stärke 64 (5) (2012) 382–391, https://doi.org/10.1002/star.201100133.
[9] P. Pineda-Gómez, A. Rosales-Rivera, M.E. Rodríguez-García, Effect of the thermo-
alkaline treatment over the thermal degradation of corn starch, Starch-Stärke 64
(10) (2012) 776–785, https://doi.org/10.1002/star.201200015.
[10] AOAC. Association of Official Analytical Chemists, Official Methods of Analysis of
A.O.A.C, 17th ed. International, Gaithersburg, MD, 2000.
[11] AACC, Approved Methods of the American Association of Cereal Chemists, 10th ed.
International, St. Paul, MN, 2000.
[12] N. Mutis González, P. Pineda Gómez, M.E. Rodríguez-García, Effect of the addition of
potassium and magnesium ions on the thermal, pasting, and functional properties
of plantain starch (Musa paradisiaca), Int. J. Biol. Macromol. 124 (2019) 41–49,
https://doi.org/10.1016/j.ijbiomac.2018.11.051.
[13] F.G. Castro-Campos, A.H. Cabrera-Ramírez, E. Morales-Sánchez, M.E. Rodríguez-
García, M. Villamiel, M. Ramos-López, M. Gaytán-Martínez, Impact of the popping
process on the structural and thermal properties of sorghum grains (Sorghum bi-
color L. Moench), Food Chem. 348 (2021), 129092, https://doi.org/10.1016/j.
foodchem.2021.129092.
[14] W. He, C. Wei, Progress in C-type starches from different plant sources, Food
Hydrocoll. 73 (2017) 162–175, https://doi.org/10.1016/j.foodhyd.2017.07.003.
[15] K. Guo, L. Zhang, X. Bian, Q. Cao, C. Wei, A-, B- and C-type starch granules coexist in
root tuber of sweet potato, Food Hydrocoll. 98 (2020), 105279, https://doi.org/10.
1016/j.foodhyd.2019.105279.
[16] C.A. Soares, F.H.G. Peroni-Okita, M. Borba Cardoso, R. Shitakubo, F.M. Lajolo, B.R.
Cordenunsi, Plantain and banana starches: granule structural characteristics explain
the differences in their starch degradation patterns, J. Agric. Food Chem. 59 (2011)
6672–6681, https://doi.org/10.1021/jf201590h.
[17] S.M. Londoño-Restrepo, R. Jeronimo-Cruz, B.M. Millán-Malo, E.M. Rivera-Muñoz,
M.E. Rodriguez-García, Effect of the nano crystal size on the x-ray diffraction pat-
terns of biogenic hydroxyapatite from human, bovine, and porcine bones, Sci. Rep.
9 (1) (2019) 5915–5923, https://doi.org/10.1038/s41598-019-42269-9.
[18] B. Gong, W. Liu, H. Tan, D. Yu, Z. Song, L.A. Lucia, Understanding shape and morphol-
ogy of unusual tubular starch nanocrystals, Carbohydr. Polym. 151 (2016) 666–675,
https://doi.org/10.1016/j.carbpol.2016.06.010.
[19] I.C. Okoli, C.M. Nwogu, I.F. Etuk, A.A. Omede, I.P. Ogbuewu, N.O. Aladi, V.M.O. Okoro,
M.N. Opara, C. Ezema, M.C. Uchegbu, B.U. Ekenyem, G.A. Anyanwu, N.J. Okeudo,
A.B.I. Udedibie, F.N. Madubuike, Plantain ash enhances dietary mineral elements ab-
sorption in pullets, Iran. J. Appl. Anim. Sci 4 (2) (2014) 351–360.
[20] H.W. Hsien-Chih, A. Sarko, The crystal structure of A-starch: is it double helical?
Carbohydr. Res. 54 (1) (1977) C3–C6, https://doi.org/10.1016/S0008-6215(00)
80566-2.
[21] H.W. Hsien-Chih, A. Sarko, The double-helical molecular structure of crystalline b-
amylose, Carbohydr. Res. 61 (1) (1978) 7–25, https://doi.org/10.1016/S0008-6215
(00)84463-8.
[22] D. Quemada, Rheology of concentrated disperse systems: II. A model for non-
newtonian shear viscosity in steady flows, Rheol. Acta 1 (1978) 632–642, https://
doi.org/10.1007/BF01522036.
[23] D. Quemada, Rheology of concentrated disperse systems: III. General features of the
proposed non-Newtonian model. Comparison with experimental data, Rheol. Acta
17 (1978) 643–653, https://doi.org/10.1007/BF01522037.
[24] D. Dufour, O. Gibert, A. Giraldo, T. Sánchez, M. Reynes, J.P. Pain, A. González, A.
Fernández, A. Díaz, Differentiation between cooking bananas and dessert bananas.
2. Thermal and functional characterization of cultivated Colombian Musaceae
(Musa sp.), J. Agric. Food Chem. 57 (17) (2009) 7870–7876, https://doi.org/10.
1021/jf900235a.
[25] A. Chávez-Salazar, L.A. Bello-Pérez, E. Agama-Acevedo, F.J. Castellanos-Galeano, C.I.
Álvarez-Barreto, G. Pacheco-Vargas, Isolation and partial characterization of starch
from banana cultivars grown in Colombia, Int. J. Biol. Macromol. 98 (2017)
240–246, https://doi.org/10.1016/j.ijbiomac.2017.01.024.
[26] J. Montoya, V.D. Quintero-Castaño, J. Lucas-Aguirre, Evaluación fisicotérmica y
reológica de harina y almidón de plátano dominico hartón (Musa paradisiaca
abb), Temas Agrarios 19 (2) (2014) 214–233.
L.J. Vega-Rojas, S.M. Londoño-Restrepo and M.E. Rodriguez-García
[27] M.E. Oseguera-Toledo, B. Contreras-Jiménez, E. Hernández-Becerra, M.E. Rodriguez-
Garcia, Physicochemical changes of starch during malting process of sorghum grain,
J. Cereal Sci. 95 (2020), 103069, https://doi.org/10.1016/j.jcs.2020.103069.
[28] N. Rincón-Londoño, L.J. Vega-Rojas, M. Contreras-Padilla, A.A. Acosta-Osorio, B.
Millan-Malo, M.E. Rodriguez-Garcia, Analysis of thermal pasting profile in corn
starch rich in amylose and amylopectin: physicochemical transformations, part I,
Int. J. Biol. Macromol. 91 (2016) 106–114, https://doi.org/10.1016/j.ijbiomac.2016.
05.070.
1731
International Journal of Biological Macromolecules 183 (2021) 1723–1731
[29] N. Rincón-Londoño, B. Millan-Malo, M.E. Rodriguez-Garcia, Analysis of thermal past-
ing profile in corn starch rich in amylose and amylopectin: physicochemical trans-
formations, part II, Int. J. Biol. Macromol. 89 (2016) 43–53, https://doi.org/10.
1016/j.ijbiomac.2016.04.057.
[30] M.D.L.Á. Cornejo-Villegas, N. Rincón-Londoño, A. Del Real-López, M.E. Rodríguez-
García, Effect of Ca2+ ions on the pasting, morphological, structural, vibrational,
and mechanical properties of corn starch–water system, J. Cereal Sci. 79 (2018)
174–182, https://doi.org/10.1016/j.jcs.2017.10.003.