Next Article in Journal
The Effect of Alginate and κ-Carrageenan on the Stability of Pickering Emulsions Stabilized by Shellac-Based Nanoparticles
Previous Article in Journal
Cellular Antioxidant Potential and Cytotoxic Activities of Extracellular Polysaccharides Isolated from Lactobacillus graminis Strain KNUAS018
 
 
Font Type:
Arial Georgia Verdana
Font Size:
Aa Aa Aa
Line Spacing:
Column Width:
Background:
Article

Extraction and Characterization of Starches from the Pulp and Peel of Native Plantain (Musa AAB Simmonds) from Two Colombian Departments

by
Juan Pablo Castañeda-Niño
1,
José Herminsul Mina-Hernández
1,* and
José Fernando Solanilla-Duque
2
1
Grupo Materiales Compuestos, Escuela de Ingeniería de Materiales, Universidad del Valle, Calle 13 No. 100-00, Cali 76001, Colombia
2
Departamento de Agroindustria, Facultad de Ciencias Agrarias, Universidad del Cauca, Sede Las Guacas, Popayán 190001, Colombia
*
Author to whom correspondence should be addressed.
Polysaccharides 2025, 6(2), 34; https://doi.org/10.3390/polysaccharides6020034
Submission received: 9 October 2024 / Revised: 24 February 2025 / Accepted: 2 April 2025 / Published: 14 April 2025
(This article belongs to the Topic Polymers from Renewable Resources, 2nd Volume)

Abstract

:
Plantain (Musa AAB Simmonds) of the Dominico hartón variety from two Colombian territories (Cauca and Risaralda) with differences in altitude was used to extract the flour and starch from the pulp and peel. The plantain of Cauca origin presented the highest yield in flour extraction. Starch extraction was based on the use of an aqueous solution of sodium metabisulfite, achieving the highest yield in starch extraction (above 80% d.b.) when using a concentration of 1.2% of sodium metabisulfite, highlighting the best performance in the plantain of Risaralda origin. In the characterization of the starches, the granules from the pulp showed a larger size, higher amylose content, lower ash content, lower water absorption and solubility capacity, higher melting enthalpy, and higher crystallinity than those obtained with the starches from the banana peel. The starch from Cauca pulp presented properties characteristic of a structure with higher hardness.

Graphical Abstract

1. Introduction

Plantain cultivation is found in tropical and subtropical areas of the planet, which are conducive to the adequate development of the mother plants and their respective bunches and other by-products. In the subcontinent of South America, being located in the areas above, it has been identified that several of the countries that comprise it (Colombia, Peru, Ecuador, Venezuela, and Brazil) are producers that contribute to the economy of the territory [1,2], contemplating the use of the bunch for the preparation and consumption of plantain, specifically its pulp is used for domestic use through cooking and/or processing in the agroindustrial sector for the production of flour and fried products, finding in plantain cultivation as the third food supplier in Colombia and the fourth largest plantain worldwide producer, generating 4,805,629 tons of plantain bunches in 2019 [3]; however, its transformation has been limited with the development of basic processed products such as flours and snacks from frying, using up to 0.5% of national production [4,5]. In this way, plantain has contributed to economic benefits in an already established production chain, despite the lack of utilization of other by-products of the crop, containing macromolecules of agroindustrial interest such as starch and lignocellulosic fibers present in the peels from the bunch, the pseudostem, the leaves, and the rachis or “acorn” [6,7,8]. The integral use of starch from plantain cultivation could contribute to the development of new processed products that participate in various sectors such as food, pharmaceuticals, cosmetics, paper, biodegradable containers, and packaging, which would contribute to strengthening national economies and the welfare of the actors in the plantain production chain [9]. The starch content present in the pulp is between 70 and 80% (d.b.), while in the peel, its presence can be identified until 50% (d.b.), while the degree of purity is higher in starch obtained from the pulp, achieving values up to 99%, while the starch from the peel achieves a purity of 70%. As for starch extraction, dry or wet methods can be used, the former being differentiated because the flour of the by-product is used to prepare a suspension with water to facilitate the separation of starch from the cake or bran, while the latter method requires the crushing of the by-product in fresh, followed by several washes with water for its respective separation [10]. In starches derived from plantains, different physicochemical, morphological, techno-functional, and rheological properties can be found that allow defining the type of processing and the type of final product to be obtained. Regarding the amylose content in the previous starches, the one coming from the pulp has values between 20.0 and 31.86% [11,12], while the amylose content in starches extracted from the peel has values between 17.0 and 32.5% [13,14]. Regarding its morphology, lenticular and semispherical shapes with diameters between 8 and 15 µm are identified, while in the elliptical shapes their lengths vary between 15 and 32 µm and the width between 10 and 15 µm, finding a superiority in their dimensions in the starch granules from the pulp with respect to those belonging to the peel [14], while in its techno-functional and rheological properties, characteristic properties of a high hardness starch for its processing are identified from the restricted absorption and solubilization in water (<2.3 g/g and <1 g/g at 60 °C, respectively), high gelatinization temperature (>70 °C), high viscosity in its gelatinization (>8 Pa.s), and retrogradation (>5 Pa.s); however, the starch from the peels generates lower viscosities in each of the stages of the pasting curves [9,14,15,16].
This research used the Dominico hartón variety from two Colombian territories (Cauca and Risaralda) as the most widely available hybrid musaceae in the country. Plantain pulp and peel were selected as the two coproducts with the greatest supply of starch, and the most appropriate method for its extraction was established, also considering its corresponding physicochemical, techno-functional, thermal, and structural characterization. The results obtained in the characterization of starch according to the extraction by-product (pulp and peel) and specific agroclimatic conditions allowed the identification the potential that these raw materials from plantains have for the development of new products in the food and non-food sectors based on the identification of the starch and amylose content, pasting curves, crystallinity, the presence of other macromolecules, among others.

2. Materials

The bunches of second- and third-quality plantain of the variety Dominico hartón were harvested between the 17th and 18th weeks after the beginning of flowering, being collected in two Colombian territories with differentiation in their altitude and agroclimatic conditions: Asociación de Productores de Finca Tradicional del Norte del Cauca (ASPROFINCA), located in the municipality of Villa Rica, Cauca (altitude: 948 m.a.s.l.), being a flat area with an average temperature of 28 °C and the Asociación de Plataneros de Santa Rosa de Cabal (ASOPLASA), Risaralda (1688 m.a.s.l.), being a mountainous area with an average temperature of 19 °C. The sodium metabisulfite used for starch extraction was acquired from Agenquímicos S.A.S. (Santiago de Cali, Valle del Cauca) in its industrial grade and was used without any modification.

3. Experimental Procedure

3.1. Extraction of Starches from Plantain Pulp and Peel

Initially, the plantain bunches were peeled, separating the peel from the pulp, on the same day of harvest to avoid advancing the ripening of the climacteric fruit, preventing the hydrolysis of starch into reducing sugars. The pulp was subjected to slicing using a knife to reduce the drying time by forced convection, using a temperature of 60 °C for 24 h, while the plantain peel was only subjected to the drying above. When a moisture content of less than 8% was achieved in the respective by-products of the bunch, the flours were obtained using a knife mill with a 0.5 mm opening screen, followed by sieving using a 100/depth sieve according to the Tyler series, obtaining particles with diameters of less than 150 µm (Figure 1a). The metabisulfite solution was mixed with the respective flours in a ratio of 5:1, respectively, using a beaker with magnetic stirring for 1 h at a temperature of 23 ± 2 °C. The resulting mixture was passed through a centrifuge to separate the slurry (starch + water) and bagasse (fibers + parenchyma). The slurry resulting from filtration was stored in 12 L containers for 24 h to achieve the starch’s sedimentation, then the supernatant was decanted, and the starch paste (wet state) was obtained. The starch paste was subjected to forced convection drying, using a temperature of 60 °C for 24 h, obtaining agglomerated starch. To reduce and standardize the particle size of the starch, a knife mill with a 0.25 mm screen was used, followed by sieving with the use of the 100 mesh/depth mesh according to the Tyler series, obtaining particles with diameters of less than 150 µm. The above procedure was carried out on the starches belonging to the plantain pulp and peel and two types of containers, a 250 mL beaker and a 4000 mL Erlenmeyer flask (Figure 1b). Considering the procedures for obtaining plantain flours and starches previously mentioned, the following samples were obtained as indicated in Table 1.
Similarly, the use of the AOAC 996.11 method was considered for the determination of the accurate starch content in the study plantain flours, using 100 mg of plantain flour with a particle size no larger than 0.5 mm, subjecting it to the mixture with 10 mL of sodium acetate (100 mM), calcium chloride (5 mM), and 0.1 mL of thermostable α-amylase with its respective vortex agitation. The above mixture was then kept in sealed test tubes in incubation at 100 °C for 15 min, followed by vortex agitation for an appropriate time depending on the starch content of the sample (5, 10, or 15 min). The sample was subjected to cooling in a thermostatic bath with a temperature of 50 °C for 5 min, and 0.1 mL of amyloglucosidases was added to establish a second incubation at 50 °C for 30 min. At the end of the incubation, 2 mL of the previous mixture was centrifuged at 13,000 r.p.m. in a microcentrifuge for 5 min. According to the method used, the sample was diluted with sodium acetate (buffer) because its starch content was higher than 10%. 0.1 mL of the previous mixture was removed, and 3 mL of the glucose determination agent was added, establishing its subsequent incubation at 50 °C for 20 min. Finally, the absorbance was measured, contrasting it with the respective absorbance of the “blank” sample [17].

3.2. Statistical Analysis

Initially, when collecting the plantain bunches from the two origins, the significant differences in the average mass and diameter of the bunch fingers in the fresh state, the pulp/peel ratio of the fingers, and the dry matter present in the plantain pulp and peel were determined by using an ANOVA and Tukey’s multiple comparison test. Having the availability of plantain flour from plantain pulp and/or peel, a unifactorial experimental design was carried out for starch extraction, considering the concentration of sodium metabisulfite as a factor and six levels (0, 0.1, 0.3, 0.6, 0.9, and 1.2%) by using a 250 mL beaker. Statistical analysis began with the determination of normality using the Shapiro–Wilk test, followed by ANOVA to determine significance (0.05) between treatments related to sodium metabisulfite concentration using SPSS IBM software, version 25. Levene’s test was used to determine the existence of equal variances, and finally, Tukey’s multiple comparison test was used. At the same time, the response variable was the amount of starch obtained in each treatment [18].
In the second stage of the starch extraction experimental design, the procedure was scaled up using a 4000 mL Erlenmeyer flask to define the concentration of sodium metabisulfite adequate for starch extraction considering the influence of stirring efficiency.

3.3. Physicochemical and Morphological Characterization of Starches from Plantain Pulp and Peel

3.3.1. Proximal Analysis

This analysis was based on five fundamental analytical procedures, where the amount of protein, ash, moisture, fiber, and lipids was determined. The determination of protein was carried out according to ISO 1871 [19], the amount of ash was determined according to ISO 2171 [20], the percentage of moisture was determined according to NTC 1776 [21], and finally, the determination of lipids and crude fiber was carried out according to NTC 668 [22].

3.3.2. pH Determination

A pH meter (Fischer Scientific, AB 150, Hampton, NY, USA) was calibrated with pH 4.0 and pH 7.0 buffer solutions to determine starch pH. Then, 20 g of starch (d.b.) was used and mixed with 100 mL of distilled water (previously boiled to remove CO2) for 15 min by magnetic stirring. The starch suspension was filtered using Whatman #1 paper (Maidstone, England, UK), supported by a funnel for pH measurement [23].

3.3.3. Morphology and Particle Size

Morphological analysis of the samples was performed on a scanning electron microscope (JEOL, JSM 6490 LV, Akishima, Japan). The samples were coated with a palladium gold layer. One milligram of each plantain’s flour and starch was used to be placed on a carbon ribbon. The images obtained were from the backscattered electron method with an accelerating power of 20 kV and a vacuum of 30 Pa in the microscope chamber, achieving magnifications of 500 and 1000× [24].

3.3.4. Amylose Content

Using previously defatted samples, the iodine colorimetric method determined the amylose content using a UV–vis spectrophotometer (UV-2550, Shimadzu, Kioto, Japan) at a wavelength of 620 nm. Initially, the sample was defatted by immersing it in analytical-grade acetone for 10 min. Ten milligrams of sample was weighed in a 100 mL flask and 10 mL of DMSO at a concentration of 99.5% w/v was added and placed in a water bath at 80 °C for 15 min. Subsequently, it was left to cool, and the gauging was completed with distilled water. One milliliter of this solution was taken, and 200 µL of acetic acid 1.0 M and 400 µL of Lugol’s solution were added. It was left to react for 20 min in the dark, and the volume was completed with 18.4 mL of distilled water. The absorbance was recorded at a wavelength of 620 nm, and the amylose content was calculated based on the highly credible calibration curve reported by Giraldo et al. [25].

3.4. Structural Properties of Starches in Plantain Pulp and Peel

3.4.1. Fourier Transform Infrared Spectrometry (ATR-FTIR)

An FTIR spectrophotometer (Shimadzu, IR Affinity-1, Kioto, Japan) with an attenuated total reflectance (ATR) accessory was used. These experiments were performed according to ASTM E1252 [26], keeping the test specimens conditioned at 50% relative humidity and 23 °C. The analysis was performed at 100 scans between 4000 and 550 cm−1 [14].

3.4.2. X-Ray Diffraction

Two grams of material with a particle size of less than 150 µm was used to form a pellet by compressing it in a rectangular mold at a temperature of 40 °C. The pellet was introduced into the diffraction chamber belonging to the X-ray diffractometer (Panalytical, X´Pert MRD, Almelo, The Netherlands), being operated at 40 kV, using a copper tube (Cukα) for the generation of radiation with a wavelength of 1.54 Å, performing a scan from 5 to 40 ° 2ϴ and with a step of 0.02 ° during 10 s. The relative crystallinity was determined like that proposed by Liu et al. [27] and based on the method of [28].

3.5. Thermal Properties of the Starches in Plantain Pulp and Peels

3.5.1. Differential Scanning Calorimetry (DSC)

Ten milligrams of each sample (starches and flours) were conditioned at a relative humidity of 50% and 23 °C, and their thermal transitions were evaluated using a TA Instruments calorimeter, DSC25, New Castle, DE, USA. Each sample was placed inside a hermetic aluminum capsule, sealed, and placed inside the thermal chamber of the DSC in an inert environment with the presence of nitrogen gas. A first heating cycle from room temperature to 90 °C was performed to erase the thermal history, followed by an isotherm at 90 °C for 5 min. Then, a 90 to −60 °C cooling cycle and an isotherm at −60 °C for 5 min were presented. Finally, a heating cycle from −60 to 250 °C was performed to determine the temperature (Tm) and the enthalpy of fusion (ΔHm) in the respective samples. The heating rate used was 10 °C/min. [29].

3.5.2. Thermogravimetric Analysis (TGA)

To study the thermal stability of starches and flours, thermogravimetric analysis equipment, TA Instruments, Q50 (New Castle, DE, USA), was used. The mass of the samples was kept between 5.0 and 8.0 mg. Each sample was subjected to a temperature range from 25 to 600 °C at a heating rate of 10 °C/min under a protective atmosphere with nitrogen gas at a 50 mL/min flow rate [30].

3.6. Techno-Functional Properties of Starches from Plantain Pulp and Peel

The water absorption index (WAI), water solubility index (WSI), and swelling power (SWP) of plantain starches were determined by weighing the sample at 0.65 g, and mixing it with 7.8 mL of distilled water, homogenizing it in a Vortex (VELP Scientifica, Classic Advanced Mixer, Usmate, Italy) using a 15 mL falcon tube for 30 s, and placing it in a water bath (Memmert, WNB14, Schwabach, Germany) for 30 min at 30 °C. The resulting sample was centrifuged (Hettich, Universal 320R centrifuge, Tuttlingen, Germany) at 5200 rpm for 10 min at 20 °C. The supernatant was removed from a Petri dish and dried at 105 °C for 24 h [31]. WAI, WSI, and SWP were calculated as shown in Equations (1)–(3).
WAI = g e l   m a s s   ( g ) s a m p l e   m a s s   ( g ) × 100   %
WSI = s o l u b l e   m a s s   ( g ) × V × 10   s a m p l e   m a s s   ( g ) × 100   %
SWP = g e l   m a s s   ( g ) s a m p l e   m a s s   ( g ) s o l u b l e   m a s s   ( g ) × 100 %

3.7. Rheological Properties of Plantain Peel and Pulp Starch

The pasting curves were measured in a rotational rheometer (TA Instruments, AR 1500, New Castle, DE, USA), using an 8% starch suspension, mixing the plantain starch with distilled water, and leaving it to stand for 1 min at room temperature, followed by using an angular rate of 78.53 rad/s inside the rheometer cylinder. The determination of the pasting properties was based on three thermal stages, starting with a heating from room temperature to 90 °C at a rate of 10 °C/min, followed by an isotherm at 90 °C for 5 min, and finally a cooling from 90 to 25 °C. The rheological parameters identified were onset temperature, peak viscosity, gelatinization temperature, breakdown viscosity, and setback viscosity [14].

3.8. Statistical Design

Finally, in the characterization of flours and starches, significant differences in pH, granule dimensions (width and length), amylose content, and techno-functional properties were determined.

4. Results and Discussions

4.1. Extraction of Starches from Plantain Pulp and Peels

4.1.1. General Characteristics of Plantain Bunch By-Products

With the availability of the by-products of the plantain bunch (pulp and peel of the plantain fingers), some physical characteristics were identified, such as peel/pulp ratio, average diameter of the plantain fingers, and dry matter content (Table 2). When peeling each of the plantain fingers, it was identified that the peel presented a participation between 41.31 and 43.28%, with dry matter between 4.25 and 5.96%. In comparison, the pulp was found to be between 56.71 and 58.69% and 24.81 and 26.19%, respectively. According to what was previously shown in the pulp/peel ratio, there is a higher proportion of pulp concerning the presence of peel in the plantain fingers in week 18 after the beginning of flowering of the mother plant. Chaves-Salazar et al. [32] report similar values for pulp content in musaceae fingers of three varieties (Dominico hartón, Gros Michel, and FHIA 20) ranging from 54.74 to 58.65%. While Montoya et al. 2014 [33] reported a fresh peel content of 36%, pulp at 64%, and dry pulp of 26.5% when evaluating plantain Dominico hartón. As for the dry matter in the two previous plantain by-products, a higher amount is reported in the pulp than in the peel. It is worth highlighting the existence of significant differences in the pulp/peel ratio and the presence of dry matter in the plantain pulp and peel. Dufour et al. 2009 [16] reported dry matter content in the pulp of musaceae (sweet bananas, sweet hybrids, cooking hybrids, cooking bananas, and plantains) between 18 and 45%. When comparing the two origins, there was a higher dry matter content in the pulp and peel of plantains from Cauca (Table 1), possibly due to a more significant stimulus for dry matter production at lower altitudes in the Dominico hartón variety. As for physical properties such as the average weight of the plantain finger, a value between 302 and 331 g was recorded, being characteristic of a second-quality fruit, since Mejía et al., 2012 [34] reported an average weight of 425 g in first-quality fruits, while the diameter at the midpoint of the fruit from the two origins presented diameters between 4.46 and 4.79 cm, being values similar to those reported by Hoyos et al. 2012 [35].

4.1.2. Starch Extraction

According to the results obtained in the one-factorial experimental design using a 250 mL beaker that allowed the extraction of starch from the plantain pulp flour (Risaralda origin), using different concentrations of sodium metabisulfite (0 to 1.2%) (Table 3). Initially, the removal of plantain starch from its respective flour was established by using only water as a solvent (yield variation between 68.35 and 80.13%), evidencing a considerable standard deviation in the extraction, leading to losses of starch being retained in the bagasse or parenchyma stored in the filter to separate it from the slurry. Montoya et al., 2014 [33] employed a mixture of water as a solvent and fresh pulp in a 1:1 ratio, respectively, for the extraction of starch from the plantain variety Dominico hartón, achieving an extraction value of 30.7%, while Flores-Gorosquera et al., 2004 [36], achieved extraction yields between 63 to 71%. The use of sodium metabisulfite solution with constant agitation allowed an increase in the amount of starch extracted when using concentrations of 0.3 and 1.2%, achieving yields between 80.21 and 81.40% (dry basis), which is higher than that obtained with water alone in the extraction. On the other hand, the increase in the concentration of the reagent promoted the increase in acidity (Table 3), possibly leading to the softening of the parenchyma that retains the starch granules. The above results were superior to those reported by De La Torre-Gutierrez et al., 2007 [18], obtaining a banana starch extraction yield with a value of 69.6% (d.b.) when using a 0.1% sodium metabisulfite solution with constant agitation for 1 h at room temperature, while Ramirez-Cortes et al., 2016 [24], achieved yields between 76 and 86% when employing a 1% sodium metabisulfite solution with agitation for 2 min and subsequent resting for 8 h. On the other hand, the treatments evaluated showed a reduction in the standard deviation in starch extraction as the concentration of sodium metabisulfite was increased until reaching a concentration of 0.6%. The quality and efficiency of plantain starch extraction using the conditions of treatments 3 and 6 were superior to most of the studies previously reported (Table 2).
The data obtained from the plantain starch extraction were subjected to a parametric test (HSD Tukey) for the sodium metabisulfite content used since most of the samples did comply with normality and equal variances. Significant differences were identified between sodium metabisulfite concentrations of 0.1 and 0.3% (sig. = 0.044), while the other treatments did not show significant differences. Based on the above, sodium metabisulfite concentrations of 0.3 and 1.2% will be considered to further adjust the scaling of banana starch extraction. By increasing the scaling of the plantain starch extraction, reductions in the respective yield can be evidenced, going from yields obtained at laboratory scale with values between 76 and 84% to industrial-scale values between 63 and 71%; a similar behavior was previously reported by Ramirez-Cortes et al. [24]. In the present experimentation, the results of treatments 3 and 6 were compared by increasing the scale, using an Erlenmeyer of 4000 mL as a container for the extraction with the respective processing conditions in the Cauca and Risaralda origins, identifying difficulty in achieving a constant and homogeneous agitation when using a solution of sodium metabisulfite at 0.3%, evidencing the sedimentation of the flour and preventing the correct agitation of the magnetic stirrer, giving two behaviors in the starch extraction yield concerning what was found in the previous processing scale, being lower in the Cauca origin (76.70% < 81.40% in d.b.). Considering the above, the real starch content and the starch amylose content in the respective flours of the two origins according to the Megazyme method (83.00 ± 0.35% in Cauca and 81.37 ± 0.64% in Risaralda), it was not possible to remove all the available starch in the Cauca origin, relating a possible opposition to its extraction to the extent that higher amylose content is found in plantain pulp starch. In contrast, in the Risaralda origin, starch and possibly some particles from other flour components such as protein and/or fiber were removed. While increasing the concentration of sodium metabisulfite to 1.2%, a continuous and homogeneous mixing was achieved, allowing higher yields in starch extraction in the two origins, since increasing the processing volume possibly increased the distribution and/or dispersion of sodium metabisulfite, contributing to a greater detachment of the granules that are initially adhered to the parenchyma in the plantain flour (Table 4) and release portions of protein and/or fiber, being subsequently separated through sieving (100 mesh according to the Tyler series). In the two concentrations of metabisulfite, a superiority of apparent starch extraction was identified in the Risaralda origin due to possible structural differences in the parenchyma, starch granules, and binding strength between the two above in the two origins. At a statistical level, based on the existence of normality and equal variances, the HSD Tukey test identified significant differences when using 0.3% sodium metabisulfite to obtain the lowest extraction yield of Cauca-origin starch with respect to the three remaining treatments (Table 4), relating a greater adherence of the respective granules with the parenchyma, making their extraction difficult. In the case of the respective flours coming from plantain peels (HCPCA and HCPR), when subjected to the starch extraction condition with higher yield in pulp flours (1.2% sodium metabisulfite solution), in the Cauca origin (ACPCA) it was possible to remove 52.69 ± 0.85%. In comparison, the Risaralda origin (ACPR) presented a value of 52.72 ± 8.16%, leaving a residual starch in the cakes (fibers and parenchyma) of the plantain peels since the total starch content in the peel flours according to the Megazyme method was 53.40 ± 1.55% (d.b.) and 59.40 ± 1.11% (d.b.), respectively.

4.2. Physicochemical, Thermal, and Structural Characterization of Flours and Starches from Plantain Coproducts

4.2.1. Proximal Analysis

The flours from plantain pulp presented ash contents between 10.13 and 13.59% and protein contents between 2.60 and 3.56%, being processed for starch extraction using sodium metabisulfite solution, generating a reduction in these contents in the respective starches with values lower than 2% (Table 5). In contrast, ash values between 12.02 and 15.38% were maintained in the starches from peels. The high ash content in the flours is related to the presence of potassium in the plantain [24,37,38,39], where the ash from the pulp flour was solubilized with the extraction water, while the retention of these minerals in the starch belonging to the peel is possibly due to the higher concentration of plantain sap, contributing to greater adhesion between the minerals and the starch granules. The proteins from the flours of both by-products were solubilized with the extraction solvent (water) used to isolate the respective starches. The crude fiber content in the flours from plantain pulp was found to range from 43.82 to 51.41%, and when starch extraction was obtained from the respective flours, values ranging from 37.29 to 50.69% were reported. Almanza-Benitez et al. [38] reported a fiber content of 55.61 ± 2.04% in a plantain flour, while García-Solís et al. [40] reported a fiber content of 62.2 ± 1.6% in a cookie containing 85% plantain flour. According to the results obtained and mentioned above, it would be expected to have the presence of starch granules between 41.31 and 54.71%. However, when testing the starch content (AOAC method 996.11) in each pulp flour, values between 81.37 and 83.00% were identified, with the Cauca origin contributing the highest proportion. The values obtained were slightly lower than those reported by Giraldo Toro et al. [25], who identified a starch content of 88.3% in plantain flour from the municipality of Puerto Tejada (Cauca). Possibly, in the method for determining crude fiber in plantain starch flours and isolates, its value includes a portion of starch granules with higher hardness in its structure in the total fiber value [41,42]. On the other hand, it can be established that starch extraction yields higher than 83.00% (Cauca) and 81.37% (Risaralda), including the blend of the respective granules with fibers or particles from the pulp parenchyma.

4.2.2. pH Determination

The flours belonging to the pulp presented pH values between a mild acidity and a neutral level (Table 5), being similar to that reported by Kumar et al. [23] and Mejía-Gutiérrez et al. [34], who found pH values between 5.0 and 6.2 in plantain varieties such as Gran Naine, Monthan, Saba, Nendran, Popoulu, and Dominico hartón, being characteristic of a native flour coming from a fruit with physiological maturation. According to the above, it is expected that the pH belonging to the starches present in the flours of the two origins is between the identified interval (5.85 to 6.01) since Paramasivam et al. [12] reported pH values between 5.85 and 6.22 in 5 varieties of plantain. However, when the respective starch extractions were carried out, a reduction in pH was generated because sodium metabisulfite contributed to the generation of this medium. The flours from the peel presented a pH characteristic of an acid medium, and the respective starch extraction contributed to a slight pH variation. At a statistical level, significant differences were identified when reducing the pH in the starches after their extraction in the respective flours; however, the previous behavior was not evident when obtaining the starch from the flour corresponding to the Risaralda plantain peel, since its initial pH presented a lower pH with respect to the 1.2% sodium metabisulfite solution.

4.2.3. Morphology and Particle Size

From the results obtained by laser granulometry, it was found that the particle sizes of the flours from the pulp were larger than those of their corresponding starches because the flour structure contains the parenchyma that contributes to the adherence of granules, generating agglomerations that increase the average value of the diameter presented in the particles (Figure 2 and Table 5). On the other hand, the SEM images show that the plantain starch granules from the different origins presented mainly elongated oval shapes with irregular ends, despite the additional identification of shapes close to a sphere (Figure 2), requiring the diameters in the length and width of the granules, generating values of sizes with greater precision than those initially obtained by laser granulometry. The averages of the two dimensions of the plantain pulp granules between the two origins did not show significant differences, maintaining their average length values between 22.90 and 23.96 µm. In contrast, the width averages were between 13.52 and 14.13 µm. When comparing the above values of pulp starches with starches from plantain peel, lower dimensions were identified without reaching a significant difference (Table 5), being a similar behavior to that obtained by Li et al., 2018 [43]. At a statistical level, significant differences were identified in width and length when comparing the starch granules from the pulp with its corresponding peel starch, with the exception of the length shown in the starches belonging to the Risaralda origin, while when comparing the two starches from the peel, they did present significant differences in their two previously mentioned dimensions; however, when contrasting between the two starches from the pulp, no significant differences were identified. The values obtained in starches from pulp and peel were close to the dimensional trend reported for the species. Otegbayo et al. [44] reported diameter variations between 9 and 25 µm (width and length, respectively) in the Agbagba variety, and Giraldo Toro et al. [25] identified an average value of the length in granules of 27.8 µm in the Dominico hartón variety; Shittu et al. [29] evaluated the varieties Nangka and Tanduk, obtaining average values of 38.97 and 23.91 µm, respectively. Likewise, Nwokocha and Williams [45] obtained values in the length of the granules between 10 and 33 µm in the white variety and between 11.22 and 41.00 µm in the yellow variety. On the other hand, when visualizing the starch granules from the peel (Cauca and Risaralda), residual fragments of the parenchyma adhered to the respective surfaces (Figure 2), probably due to the greater presence of plantain sap in its structure, which is responsible for keeping the fibers or particles of the parenchyma adhered to the surface of the granules during the extraction process.

4.2.4. Amylose Content

The amylose content in pulp starches presented values higher than 20%, characteristic of type II resistant starches [46,47,48], considering a higher value in Cauca origin (Table 5). Giraldo Toro et al. [25] reported amylose contents between 20.4 and 23.4% in flour from Dominico hartón variety pulp, while Otegbayo et al. [44] identified amylose contents in pulp starch between 23 and 25%. On the other hand, Nasrin et al. [14] presented the highest amylose content values in pulp (39.8%) and plantain peel (32.5%) starches. However, the apparent hardness character was not evident in starches from peels in the two origins since amylose contents were lower than those presented in the respective pulps with values below 19%, a behavior like that found by Nasrin et al. [14]. At a statistical level, no significant differences were identified in the amylose content between the two starches from the peel; however, the starches from the pulps, apart from presenting a higher amylose content with respect to those from the peels, presented significant differences, highlighting the greater differentiation provided by the Cauca origin.

4.3. Structural Properties of Starches in Plantain Pulp and Peel

4.3.1. Fourier Transform Infrared Spectrometry (ATR-FTIR)

The spectra of each of the starches and flours are distributed in three regions (Figure 3): the band of tensile stretching generated by O-H bonds (3560–3000 cm−1) and C-H bonds (3000–2800 cm−1) and the characteristic region of starch (1600–650 cm−1) [14]. The starches and their respective plantain flours of the two origins presented a broad band between 3303.24 and 3275.13 cm−1, corresponding to symmetric and asymmetric stress vibrations due to the O-H bonds present in the starch structure, being causative of the presence of water adsorbed on the surface of the starch granule [23,49]. The band’s bandwidth indicates the presence of intermolecular hydrogen bonds [13]. The O-H above bonds have a strain band between 1639.56 and 1637.56 cm−1 in pulp flours, between 1646.32 and 1635.71 cm−1 in pulp starches, and between 1629.85 and 1621.24 cm−1 in peel starches (Figure 3) [14]. The second stress band corresponding to C-H bonds in plantain starches and flours is found between 2920 and 2930 cm−1, while the respective vibrational bands were identified between 1326 and 1413 cm−1. In the last region, the characteristic band of carbohydrates [13] is found, comprised of three peaks between the interval of 995 to 1149 cm−1, generating vibrations of tension of the C-O-C (ether) bonds and deformation of the O-H, since there are C-O interactions with different chemical environments [13,14,23,49]. Although the above signals were present in all samples, the pulp flour and starch from the Risaralda origin peel presented a peak between 1733 and 1735 cm−1, relating the presence of type I amide bonds to the presence of proteins [14]. However, Ferreira-Villadiego et al. [13] reported signals present between 1500 and 2000 cm−1, relating to the presence of double bonds (alkene) in the structure of the starch molecule.

4.3.2. X-Ray Diffraction

With the diffractograms, it was possible to identify a semi-crystalline structure in the starches (pulp and peel) and plantain pulp flours of the Dominico hartón variety from the two origins, although differences in the type of crystallinity pattern were evidenced; type B structure was found in the by-products of the Risaralda origin and the starch from the plantain peel of the Cauca origin, while the flour and starch from the pulp of the Cauca origin presented the type C crystallinity pattern (Figure 4 and Table 5). The type B pattern is characteristic in starches with high amylose content, such as musaceae and potatoes, presenting a hexagonal unit cell. In contrast, the type C crystalline structure presents a mixture of type A and B crystallites, finding monoclinic unit cells (giving greater packing in the structure) inside the granule and hexagonal unit cells surrounding the previous structures to form the starch granule, being a polymorphic structure [29,50,51]. At the same time, De La Torre-Gutierrez et al. [18] reported a C-type structure constituted by hexagonal unit cells in the interior and monoclinic unit cells in the periphery of the starch granule. Other reports have identified different types A [29], B [12,36,43,46,52], and C [12,23,51,52,53,54] crystalline structures in plantain starches. According to the present investigation, using flour and starch from plantain pulp and peel, the three crystallinity patterns can be found when considering the same species and variety. Another relevant factor in the changes in the crystallinity pattern in starches was the agroclimatic differences to which plantain is exposed [55]. A common characteristic in plantain flour and starch samples is related to identifying three peaks with average intensity between 7.49 and 11.25° 2ϴ (Table 5), similar to that evidenced by Soares et al. [53] when using Terra and Figo plantain varieties. At the same time, in other reports, such signals are identified with low-intensity peaks when evaluating potato, corn, and plantain starches [29,43,46,54]. However, in the investigations of Agama-Acevedo et al. [37] and Monroy et al. [56], similar structural behaviors were not evidenced in type A patterns belonging to corn starch and type C in that corresponding to cassava.
On the other hand, it should be highlighted that the higher intensity at angles 15 and 17° 2ϴ presented in the diffractograms of plantain flours and starches, relating the highest values of relative crystallinity concerning what is reported in the literature [23,43,49,50], since the plantain pulp flours achieved values between 43.67 and 50.77%, pulp starches between 45.78 and 46.09%, and peel starches between 33.39 and 37.02% (Table 5), while the relative crystallinity of starches from other botanical sources such as maize (14 to 39%), wheat (27 to 36%), waxy rice (38%), potato (23 to 25%), cassava (13 to 38%), and musaceae (2 to 30%), among others. Starches with higher amylopectin content are expected to contribute to the crystalline phase’s conformation, as evidenced by X-ray diffraction [50,51,57,58,59,60]. However, starches such as those found in the peels presented the lowest crystallinity contents in their structure despite containing a higher proportion of amylopectin, unlike starches from plantain pulp that presented the highest relative crystallinity despite containing a higher proportion of amylose. Zhu (2015) [61] reported that amylopectin chains interact among themselves and with water molecules through secondary bonds when found inside the starch granule. However, the length of these polymeric chains defines the preference for interaction with other amylopectin chains or with water, establishing greater affinity with neighboring amylopectin chains of greater length [62]. Despite considering the above, Shittu et al. [29] reported a behavior similar to that manifested in the present investigation, obtaining relative crystallinity values of 61.1% in a banana starch variety “Nangka” when presenting an amylose content of 31.79% concerning “Tanduk” banana starch with values of 52.1 and 26.08%, respectively, relating higher crystallinity to higher amylose content in plantain starch due to a possible interaction of the amylose chains with the long and short chains of amylopectin. This interaction was also evidenced in the Grand Naine, Nendran, and Saba plantain varieties, presenting relative crystallinities and amylose contents of 21.19 and 10.70%, 25.03 and 13.46%, and 52.02 and 19.57%, respectively [12,23].

4.4. Thermal Properties of the Starches in Plantain Pulp and Peels

The thermal analysis of starches considers the size and shape of granules, the participation of the crystalline phase in their structure, and the chain length of amylopectin [29], involving the melting temperature (Tm), the enthalpy of fusion (ΔHm), and the thermal degradation temperature (Td) in the different plantain by-products (Table 5). When comparing the Tm, ΔHm, and Td of the flours concerning the pulp starches in the Cauca and Risaralda origins, the other macromolecules (proteins and fibers) present in the flour contributed to the protection of the starch granule from melting by generating higher melting temperatures; lower enthalpy was required in the melting of the granules due to their lower concentration and lower thermal degradation temperatures since starch has greater thermal stability concerning the other macromolecules present in the flours. While in the Tm and ΔHm of starches belonging to the two origins, a proportionality was identified concerning the amylose content, achieving the highest values in the Cauca origin. According to the above, the DSC thermograms relate a possible influence of amylose on the crystallinity present in the starch granules; in this sense, Shittu et al. [29] reported a higher melting temperature and relative crystallinity index in the Nangka variety plantain starch concerning the Tanduk variety, presenting amylose contents of 31.79 and 26.08%, respectively. Likewise, Li et al. [43] found higher temperatures and melting enthalpies in plantain starches as the amylose content increases. Bi et al. [52] mentioned that the increase in enthalpy in plantain starches is due to the presence of resistant starches. A similarity in Tm was evidenced when comparing such thermal properties between pulp and peel starches. At the same time, higher heat energy was required in pulp granules for melting from the higher amylose content. Finally, in the thermal degradation of starches from the TGA, greater thermal stability was evidenced in starches from pulp with higher amylopectin content, highlighting the higher thermal degradation temperature given by the starch from Risaralda pulp origin with a value of 316.92 °C. The above-mentioned is related to that reported by Liu et al. [63], where they evaluated four types of corn starch with different amylose contents (0 to 80%), identifying greater thermal stability of starch with higher amylopectin content (330 °C in waxy starch) concerning starches with lower amylopectin content (317 °C in starch with 20% amylopectin), since it provides greater length in the polymeric chain and greater molecular weight for breaking bonds at high temperature. In the case of starches from peels, the superiority of Td in the Risaralda origin is maintained; however, its values are lower than those of starches from the two pulps, probably due to impurities.

4.5. Techno-Functional Properties of Starches from Plantain Pulp and Peel

In the WAI and SWP, the lower water retention and expansion capacity of the starch granule from the Cauca origin pulp is evidenced by the higher amylose content (Table 5). In the case of the Risaralda origin, the highest values of WAI, WSI, and SWP were evidenced, relating to a starch of lower hardness in its structure from the lower amylose content, highlighting a higher degree of water solubility of the starch from the peel. In this sense, Olatunde et al. [64] reported that those starches with higher WSI values have higher amylopectin content. The higher water solubility index was evidenced in the peel starches compared to the respective pulp starches due to the lower amylose content and smaller granule size. Therefore, amylopectin contributes to solubilization with water. Otegbayo et al. [44] mentioned that starches with larger sizes present lower intermolecular adhesion, and those with higher amylose content contribute to the reinforcement of the internal structure of the granule, generating an increase in the restriction of dimensional changes of starches from pulp when exposed to water. Li et al. [43] reported similar behavior, achieving higher solubility in peel starches than in plantain pulp. This shows differences in the techno-functional properties of starches belonging to different by-products of the same origin (Table 5). At a statistical level, the WAI and SWP showed the same behavior, identifying significant differences between the Cauca pulp starch, the Cauca peel starch, and the Risaralda starches, considering that the latter two starches have no significant differences, while in the WSI, there were significant differences between the four starches.

4.6. Rheological Properties of Plantain Pulp and Peel Starches

Figure 5 shows the pasting curves of plantain starches from pulp and peel, showing their different stages (onset, maximum viscosity, gelatinization temperature, breakdown, and setback). This rheological behavior depends on several parameters, such as the amounts of amylose and amylopectin, granule size, and amylopectin branching size [65]. In most starches belonging to cereals, the gelatinization peak, presenting high viscosity at lower gelatinization temperature, is related to the lower concentration of amylose in the starch [66]. However, Dufour et al. [16] reported a weak relationship between gelatinization temperature and amylose content after evaluating 23 starches from the pulps of different musaceae, which was opposite to the behavior pattern already identified in cereal starches since there is a directly proportional relationship between the increase in viscosity as the amylose content increases in starches from bananas and plantains. In the present investigation, the highest viscosity values at gelatinization peak, breakdown, and setback were reported for starches from pulp concerning starches from the peel. Nasrin et al. [14] found similar behavior in gelatinization viscosities and breakdown when evaluating starches from the pulp and peel of the Kluai Namwa plantain variety, where the lower viscosity values evidenced in peel starches were due to the possible presence of particles that do not contribute to gelatinization such as fibers, protein, and parenchyma. Pulp starch of Cauca origin gave the highest viscosity, relating the starch with the highest hardness or apparent resistance according to the techno-functional analysis and due to its higher amylose content. In the case of starches from the peels, possibly, the viscosity behavior resembles the viscosity pattern in cereals, evidencing higher viscosity in the starch from the Risaralda origin peel, presenting lower amylose content. It is also necessary to consider the difference in the size of the starch granules from the two origins peels, evidencing the lower gelatinization temperature, higher gelatinization viscosities, breakdown, and setback from the larger size in the Risaralda origin. The onset temperature relates to the beginning of water absorption of the starch granules and the increase in their dimensions, relating to the increase in the viscosity of the starch solution. In this case, the starches from Risaralda plantain pulp and peel presented the onset temperature at 66.80 and 63.90 °C, respectively, while the starches from Cauca presented values above 71.60 °C (Table 5). The pasting or gelatinization temperature relates to the beginning of granule breakage after maximum swelling following water absorption, achieving temperatures between 86.50 and 91.60 °C, with values higher than those obtained by Dufour et al. [16], who obtained temperatures between 75.2 and 77.4 °C when evaluating different plantain varieties (Africa, Dominico, Dominico hartón, hartón, Cubano blanco, and maqueño), while Nwokocha and Williams [45] obtained values between 61 and 68 °C. Otegbayo et al. [44] mentioned that starches with higher gelatinization temperature and viscosity values indicate that their granules have greater resistance to swelling and rupture. Upon breakdown, starch granules progress with their breakdown or destructuring as the heating time advances at 90 °C, evidencing a drop in viscosity due to the release or leaching of amylose, followed by the melting of amylopectin. In this case, the greatest drop in viscosity occurred in the pulp starches due to the release of amylose from the granule; however, the Cauca origin presented greater viscosity in the breakdown, relating a greater proportion of unfractured granules to the presence of bonds of greater binding strength inside the granules. In the final part of the analysis (setback), the higher speed of the increase in viscosity in the pulp starches was evidenced since the higher amylose content manifested recrystallization or retrogradation in the short term. Another parameter to consider in the lower speed of viscosity increase in the setback corresponding to plantain peel starches is the presence of molecules other than starch [14,44]. Considering the application of starches from plantain pulp and peel according to their amylose content, granule sizes, crystallinity, techno-functional properties and rheological behavior, starches from pulp would generate greater torque during extrusion processing to obtain transformed products destined for the food and non-food sectors [14]. Retrogradation in pulp starches can occur more quickly, relating to texture changes in the short-term storage of the transformed products [67] with respect to what plantain peel starches could suffer. The lower amylose content in starch from the peel has the potential for the development of biobased materials such as flexible films from its lower amylose content and lower values in rheological properties, since Castañeda-Niño [68] achieved lower thicknesses and greater tensile properties in a flexible film from cassava starch.

5. Conclusions

According to the research conducted on plantain flours and starches of the Dominico hartón variety, considering two Colombian origins, several characteristics and differentiating properties were identified in the extraction of flours and starches and their physicochemical, techno-functional, thermal, and structural characterization. The altitude and agroclimatic conditions of the site for the establishment and development of the Dominico hartón crop are relevant to achieving higher yields in starch extraction. The starch extraction procedure with the highest yields was generated by using a concentration of 0.3 and 1.2% of sodium metabisulfite in a 250 mL container; however, when changing the scale for the starch extraction, moving to a 4000 mL container, a high viscosity of the increase in the volume of the water–flour mixture was identified, making homogeneous stirring difficult when using 0.3% of metabisulfite, requiring an increase in the sodium metabisulfite content to 1.2% to increase its dispersion in the flour and achieve greater detachment of the granules in the parenchyma structure. The extraction yields of plantain starch were high due to particles coming from the parenchyma, which found a more significant presence of this impurity in the starch of plantain peels. Any possible detachments of the parenchyma remaining in the starch can be corrected by screening using a 100 and/or 200 mesh. As reported by DSC, TGA, XRD, pasting curves, and techno-functional properties of pulp starches present higher hardness, requiring more processing energy than peel starches. The amylose content was higher in pulp starches, being one of the factors responsible for the hardness of these starches, highlighting what was evidenced in the Cauca origin. Another factor responsible for the hardness of the previous starches is related to a higher degree of intermolecular interaction of the amylopectin and amylose chains, contributing to a higher degree of crystallinity.

Author Contributions

Conceptualization, J.P.C.-N., J.H.M.-H. and J.F.S.-D.; methodology, J.P.C.-N. and J.H.M.-H.; investigation, J.P.C.-N. and J.H.M.-H.; writing—original draft preparation, J.P.C.-N. and J.H.M.-H.; and writing—review and editing, J.P.C.-N., J.H.M.-H. and J.F.S.-D. All authors have read and agreed to the published version of the manuscript.

Funding

This research has been funded by Vicerrectoría de Investigaciones de la Universidad del Valle through the Convocatoria Interna 123-2020 (C.I. 3233) and Convocatoria de apoyo a estudiantes de Doctorado 149-2023 (C.I. 21243).

Institutional Review Board Statement

Not applicable.

Data Availability Statement

Data are contained within the article.

Acknowledgments

The authors acknowledge the Escuela de Ingeniería de Materiales and Departamento de Química of the Universidad del Valle and the Centro de Desarrollo Tecnológico Agroindustrial (CDTA-UTP) of the Universidad Tecnológica de Pereira.

Conflicts of Interest

The authors declare no conflicts of interest.

References

  1. Dita, M.; Garming, H.; Den Bergh, I.; Staver, C.; Lescot, T. Banana in Latin America and the Caribbean: Current state challenges and perspectives. Acta Hortic. 2013, 986, 365–380. [Google Scholar] [CrossRef]
  2. Jaramillo, R. Banana and Plantain Production in Latin America and the Caribbean. In Proceedings of the International Workshop, Cairns, Australia, 13–17 October 1986. Banana and Plantain Breeding Strategies: ACIAR No. 21, 197p. [Google Scholar]
  3. Minagricultura. CADENA DE PLÁTANO; 2020. Available online: https://sioc.minagricultura.gov.co/Platano/Documentos/2020-03-31%20Cifras%20Sectoriales.pdf (accessed on 24 February 2025).
  4. CORPOICA. El cultivo de Plátano; 1999. Available online: https://repository.agrosavia.co/handle/20.500.12324/2095 (accessed on 24 February 2025).
  5. Arizabaleta, C.; Giraldo, A. Diversificación de Productos Agroindustriales Colombianos para Exportación; Colegio de Estudios Superiores de Administración—CESA: Bogota, Colombia, 2018. [Google Scholar]
  6. Gómez Soto, J.A.; Sánchez Toro, Ó.J.; Matallana Pérez, L.G. Processes of transformation: Perspective of use for the residues of the plantain agro-industry. Prod. Limpia 2021, 16, 6–30. [Google Scholar]
  7. Mohapatra, D.; Mishra, S.; Meda, V. Plantains and their postharvest uses: An overview. Stewart Postharvest Rev. 2009, 5, 1–11. [Google Scholar]
  8. Serna-Jiménez, J.A.; Siles López, J.Á.; De Los Ángeles Martín Santos, M.; Chica Pérez, A.F. Exploiting waste derived from Musa spp. processing: Banana and plantain. Biofuels Bioprod. Biorefining 2023, 17, 1046–1067. [Google Scholar] [CrossRef]
  9. Castañeda-Niño, J.P.; Mina-Hernandez, J.H.; Valadez-González, A. Potential uses of Musaceae wastes: Case of application in the development of bio-based composites. Polymers 2021, 13, 1844. [Google Scholar] [CrossRef] [PubMed]
  10. Hernández-Carmona, F.; Morales-Matos, Y.; Lambis-Miranda, H.; Pasqualino, J. Starch extraction potential from plantain peel wastes. J. Environ. Chem. Eng. 2017, 5, 4980–4985. [Google Scholar] [CrossRef]
  11. Mestres, C.; Taylor, M.; McDougall, G.; Arufe, S.; Tran, T.; Nuwamanya, E.; Dufour, D.; Nakitto, M.; Meghar, K.; Rinaldo, D.; et al. Contrasting Effects of Polysaccharide Components on the Cooking Properties of Roots, Tubers and Bananas. J. Sci. Food Agric. 2024, 104, 4652–4661. [Google Scholar] [CrossRef]
  12. Paramasivam, S.K.; Saravanan, A.; Narayanan, S.; Shiva, K.N.; Ravi, I.; Mayilvaganan, M.; Pushpa, R.; Uma, S. Exploring differences in the physicochemical, functional, structural, and pasting properties of banana starches from dessert, cooking, and plantain cultivars (Musa spp.). Int. J. Biol. Macromol. 2021, 191, 1056–1067. [Google Scholar] [CrossRef]
  13. Ferreira-Villadiego, J.; García-Echeverri, J.; Vidal, M.V.; Pasqualino, J.; Meza-Castellar, P.; Lambis-Miranda, H.A. Chemical modification and characterization of starch derived from plantain (Musa paradisiaca) peel waste, as a source of biodegradable material. Chem. Eng. Trans. 2018, 65, 763–768. [Google Scholar]
  14. Nasrin, T.A.A.; Noomhorm, A.; Anal, A.K. Physico-Chemical Characterization of Culled Plantain Pulp Starch, Peel Starch, and Flour. Int. J. Food Prop. 2015, 18, 165–177. [Google Scholar] [CrossRef]
  15. Torres-Vargas, O.L.; Gaytan-Martinez, M.; Fernanda, C.C.; Millán-Malo, B.M.; Rodriguez-Garcia, M.E. Changes in the Physicochemical Properties of Isolated Starch and Plantain (Musa AAB Simmonds) Flours for Early Maturity Stage. Heliyon 2023, 9, e18939. [Google Scholar] [CrossRef]
  16. Dufour, D.; Gibert, O.; Giraldo, A.; Sánchez, T.; Reynes, M.; Pain, J.P.; González, A.; Fernández, A.; Díaz, A. Differentiation between cooking bananas and dessert bananas. 2. Thermal and functional characterization of cultivated Colombian Musaceae (Musa sp.). J. Agric. Food Chem. 2009, 57, 7870–7876. [Google Scholar] [CrossRef] [PubMed]
  17. Megazyme Total Starch Assay Kit (AA/AMG). Available online: https://www.megazyme.com/total-starch-assay-kit (accessed on 24 February 2025).
  18. De La Torre-Gutierrez, L.; Torruco-Uco, J.G.; Castellanos-Ruelas, A.; Chel-Guerrero, L.A.; Betancur-Ancona, D. Isolation and structure investigations of square banana (Musa balbisiana) starch. Starch-Stärke 2007, 59, 326–333. [Google Scholar] [CrossRef]
  19. ISO 1871:2009; Food and Feed Products—General Guidelines for the Determination of Nitrogen by the Kjeldahl Method. International Organization for Standardization ISO: Geneva, Switzerland, 2021.
  20. ISO 2171:2010; Cereals, Pulses and by-Products—Determination of Ash Yield by Incineration. International Organization for Standardization ISO: Geneva, Switzerland, 2023.
  21. Norma Técnica Colombiana NTC1776:2019; Test Method to Determine the Total Evaporable Moisture Content of Aggregate by Drying. NTC: Bogotá, Colombia, 2019.
  22. Norma Técnica Colombiana NTC 668:1973; Alimentos y Materias Primas Determinación de los Contenidos de Grasa y Fibra Cruda. NTC: Bogotá, Colombia, 2002.
  23. Kumar, P.S.; Saravanan, A.; Sheeba, N.; Uma, S. Structural, functional characterization and physicochemical properties of green banana flour from dessert and plantain bananas (Musa spp.). LWT—Food Sci. Technol. 2019, 116, 108524. [Google Scholar] [CrossRef]
  24. Ramirez-Cortes, R.; Bello-Pérez, L.A.; Gonzalez-Soto, R.A.; Gutierrez-Meraz, F.; Alvarez-Ramirez, J. Isolation of plantain starch on a large laboratory scale. Starch-Starke 2016, 68, 488–495. [Google Scholar] [CrossRef]
  25. Giraldo Toro, A.; Gibert, O.; Ricci, J.; Dufour, D.; Mestres, C.; Bohuon, P. Digestibility prediction of cooked plantain flour as a function of water content and temperature. Carbohydr. Polym. 2015, 118, 257–265. [Google Scholar] [CrossRef] [PubMed]
  26. ASTME1252-98; Standard Practice for General Techniques for Obtaining Infrared Spectra for Qualitative Analysis. ASTM: West Conshohocken, PA, USA, 2021.
  27. Liu, H.; Yu, L.; Chen, L.; Li, L. Retrogradation of corn starch after thermal treatment at different temperatures. Carbohydr. Polym. 2007, 69, 756–762. [Google Scholar] [CrossRef]
  28. Nara, S.; Komiya, T. Studies on the Relationship Between Water-satured State and Crystallinity by the Diffraction Method for Moistened Potato Starch. Starch-Stärke 1987, 35, 407–410. [Google Scholar] [CrossRef]
  29. Shittu, R.; Lasekan, O.; Karim, R.; Sulaiman, R. Plantain-starch: Microstructural, physicochemical, and morphological characteristics of two cultivars grown in Malaysia. Starch-Starke 2016, 68, 1187–1195. [Google Scholar] [CrossRef]
  30. Rodriguez, L. Elaboración de un Material Biocompuesto a Partir de la Fibra de Plátano. Master’s Thesis, Universidad Nacional de Colombia, Bogotá, Colombia, 2014. [Google Scholar]
  31. Padhi, S.; Dwivedi, M. Physico-chemical, structural, functional and powder flow properties of unripe green banana flour after the application of Refractance window drying. Future Foods 2022, 5, 100101. [Google Scholar] [CrossRef]
  32. Chavez-Salazar, A.M.; Castellanos-Galeano, F.J.; Martinez-Hernandez, L.J. Effect of process variables in the production of fried green plantain in vacuum. Vitae 2017, 24, 38–46. [Google Scholar] [CrossRef]
  33. Montoya, J.; Quintero, V.D.; Lucas, J.C. Thermal and rheological evaluation of flour and starch from banana dominico harton (Musa paradisiaca ABB). Temas Agrar. 2014, 19, 214–233. [Google Scholar] [CrossRef]
  34. Mejía-Gutiérrez, L.; Giraldo-Gómez, G.; Ramírez-Ramírez, D. Efecto de la edad de cosecha en las características poscosecha del plátano Dominico-Hartón (Musa AAB Simmonds). Acta Agron. 2012, 61, 345–352. [Google Scholar]
  35. Hoyos-Leyva, J.D.; Jaramillo-Jiménez, P.A.; Giraldo-Toro, A.; Dufour, D.; Sánchez, T.; Lucas-Aguirre, J.C. Physical, morphological characterization and evaluation of pasting curves of Musa spp. Acta Agron. 2012, 61, 214–229. [Google Scholar]
  36. Flores-Gorosquera, E.; García-Suárez, F.J.; Flores-Huicochea, E.; Núñez-Santiago, M.C.; González-Soto, R.A.; Bello-Pérez, L.A. Yield of starch extraction from plantain (Musa paradisiaca). Pilot plant study. Acta Cient. Venez. 2004, 55, 86–90. [Google Scholar] [PubMed]
  37. Agama-Acevedo, E.; Bello-Pérez, L.A.; Pacheco-Vargas, G.; Evangelista-Lozano, S. Inner structure of plantain starch granules by surface chemical gelatinization: Morphological, physicochemical and molecular properties. Rev. Mex. Ing. Química 2015, 14, 73–80. [Google Scholar]
  38. Almanza-Benitez, S.; Osorio-Díaz, P.; Méndez-Montealvo, G.; Islas-Hernández, J.J.; Bello-Perez, L.A. Addition of acid-treated unripe plantain flour modified the starch digestibility, indigestible carbohydrate content and antioxidant capacity of semolina spaghetti. LWT—Food Sci. Technol. 2015, 62, 1127–1133. [Google Scholar] [CrossRef]
  39. Flores-Silva, P.C.; Rodriguez-Ambriz, S.L.; Bello-Pérez, L.A. Gluten-Free Snacks Using Plantain-Chickpea and Maize Blend: Chemical Composition, Starch Digestibility, and Predicted Glycemic Index. J. Food Sci. 2015, 80, C961–C966. [Google Scholar] [CrossRef]
  40. García-Solís, S.E.; Bello-Pérez, L.A.; Agama-Acevedo, E.; Flores-Silva, P.C. Plantain flour: A potential nutraceutical ingredient to increase fiber and reduce starch digestibility of gluten-free cookies. Starch-Starke 2018, 70, 1700107. [Google Scholar] [CrossRef]
  41. Fuentes-Zaragoza, E.; Riquelme-Navarrete, M.J.; Sánchez-Zapata, E.; Pérez-Álvarez, J.A. Resistant starch as functional ingredient: A review. Food Res. Int. 2010, 43, 931–942. [Google Scholar] [CrossRef]
  42. Saura Calixto, P.F.; Abla, R. Resistant starch: An indigestible fraction of foods. Grasas Aceites 1991, 42, 239–242. [Google Scholar] [CrossRef]
  43. Li, M.; Tian, X.; Jin, R.; Li, D. Preparation and characterization of nanocomposite films containing starch and cellulose nanofibers. Ind. Crops Prod. 2018, 123, 654–660. [Google Scholar] [CrossRef]
  44. Otegbayo, B.; Lana, O.; Ibitoye, W. Isolation And Physicochemical Characterization Of Starches Isolated From Plantain (Musa Paradisiaca) And Cooking Banana (Musa Sapientum). J. Food Biochem. 2010, 34, 1303–1318. [Google Scholar] [CrossRef]
  45. Nwokocha, L.M.; Williams, P.A. Some properties of white and yellow plantain (Musa paradisiaca, Normalis) starches. Carbohydr. Polym. 2009, 76, 133–138. [Google Scholar] [CrossRef]
  46. Bertolini, A. Starches Characterization, Properties and Applications; CRC Press Taylor & Francis Group: Boca Raton, FL, USA, 2010. [Google Scholar]
  47. Birt, D.F.; Boylston, T.; Hendrich, S.; Jane, J.L.; Hollis, J.; Li, L.; McClelland, J.; Moore, S.; Phillips, G.J.; Rowling, M.; et al. Resistant starch: Promise for improving human health. Adv. Nutr. 2013, 4, 587–601. [Google Scholar] [CrossRef] [PubMed]
  48. Janssen, L.; Moscicki, L. Thermoplastic Starch A Green Material for Various Industries; Wiley-VCH Verlag: Weinheim, Germany, 2009. [Google Scholar]
  49. Pelissari, F.M.; Andrade-Mahecha, M.M.; Sobral, P.J.D.A.; Menegalli, F.C. Isolation and characterization of the flour and starch of plantain bananas (Musa paradisiaca). Starch-Starke 2012, 64, 382–391. [Google Scholar] [CrossRef]
  50. Dome, K.; Podgorbunskikh, E.; Bychkov, A.; Lomovsky, O. Changes in the crystallinity degree of starch having different types of crystal structure after mechanical pretreatment. Polymers 2020, 12, 641. [Google Scholar] [CrossRef]
  51. Lopez-Rubio, A.; Flanagan, B.M.; Gilbert, E.P.; Gidley, M.J. A novel approach for calculating starch crystallinity and its correlation with double helix content: A combined XRD and NMR study. Biopolymers 2008, 89, 761–768. [Google Scholar] [CrossRef]
  52. Bi, Y.; Zhang, Y.; Gu, Z.; Cheng, L.; Li, Z.; Li, C.; Hong, Y. Effect of ripening on in vitro digestibility and structural characteristics of plantain (Musa ABB) starch. Food Hydrocoll. 2019, 93, 235–241. [Google Scholar] [CrossRef]
  53. Soares, C.A.; Peroni-Okita, F.H.G.; Cardoso, M.B.; Shitakubo, R.; Lajolo, F.M.; Cordenunsi, B.R. Plantain and banana starches: Granule structural characteristics explain the differences in their starch degradation patterns. J. Agric. Food Chem. 2011, 59, 6672–6681. [Google Scholar] [CrossRef]
  54. Waliszewski, K.N.; Aparicio, M.A.; Bello, L.A.; Monroy, J.A. Changes of banana starch by chemical and physical modification. Carbohydr. Polym. 2003, 52, 237–242. [Google Scholar] [CrossRef]
  55. Ekafitri, R.; Kumalasari, R.; Suryani, Y.; Acahyadi, N.S.; Desnilasari, D.; Mayasti, N.K.I.; Surahman, D.N. Characteristics of flour plantain: Use of fruit peels and ripening fruit stages. Emir. J. Food Agric. 2021, 33, 980–991. [Google Scholar] [CrossRef]
  56. Monroy, Y.; Rivero, S.; García, M.A. Microstructural and techno-functional properties of cassava starch modified by ultrasound. Ultrason. Sonochemistry 2018, 42, 795–804. [Google Scholar] [CrossRef]
  57. Cheetham, N.W.H.; Tao, L. Variation in crystalline type with amylose content in maize starch granules: An X-ray powder diffraction study. Carbohydr. Polym. 1998, 36, 277–284. [Google Scholar] [CrossRef]
  58. Chung, H.J.; Liu, Q.; Lee, L.; Wei, D. Relationship between the structure, physicochemical properties and in vitro digestibility of rice starches with different amylose contents. Food Hydrocoll. 2011, 25, 968–975. [Google Scholar] [CrossRef]
  59. Fekete, E.; Bella, É.; Csiszár, E.; Móczó, J. Improving physical properties and retrogradation of thermoplastic starch by incorporating agar. Int. J. Biol. Macromol. 2019, 136, 1026–1033. [Google Scholar] [CrossRef]
  60. Kong, X.; Zhu, P.; Sui, Z.; Bao, J. Physicochemical properties of starches from diverse rice cultivars varying in apparent amylose content and gelatinisation temperature combinations. Food Chem. 2015, 172, 433–440. [Google Scholar] [CrossRef] [PubMed]
  61. Zhu, F. Composition, structure, physicochemical properties, and modifications of cassava starch. Carbohydr. Polym. 2015, 122, 456–480. [Google Scholar] [CrossRef]
  62. Agarwal, S. Major factors affecting the characteristics of starch based biopolymer films. Eur. Polym. J. 2021, 160, 110788. [Google Scholar] [CrossRef]
  63. Liu, X.; Yu, L.; Xie, F.; Li, M.; Chen, L.; Li, X. Kinetics and mechanism of thermal decomposition of corn starches with different amylose/amylopectin ratios. Starch-Starke 2010, 62, 139–146. [Google Scholar] [CrossRef]
  64. Olatunde, G.O.; Arogundade, L.K.; Orija, O.I. Chemical, functional and pasting properties of banana and plantain starches modified by pre-gelatinization, oxidation and acetylation. Cogent Food Agric. 2017, 3, 1283079. [Google Scholar] [CrossRef]
  65. Srichuwong, S.; Sunarti, T.C.; Mishima, T.; Isono, N.; Hisamatsu, M. Starches from different botanical sources II: Contribution of starch structure to swelling and pasting properties. Carbohydr. Polym. 2005, 62, 25–34. [Google Scholar] [CrossRef]
  66. Yuan, T.Z.; Ai, Y. Pasting and gelation behaviors and in vitro digestibility of high-amylose maize starch blended with wheat or potato starch evaluated at different heating temperatures. Food Hydrocoll. 2022, 131, 107783. [Google Scholar] [CrossRef]
  67. Chaudhary, A.L.; Torley, P.J.; Halley, P.J.; McCaffery, N.; Chaudhary, D.S. Amylose Content and Chemical Modification Effects on Thermoplastic Starch from Maize—Processing and Characterisation Using Conventional Polymer Equipment. Carbohydr Polym 2009, 78, 917–925. [Google Scholar] [CrossRef]
  68. Castañeda Niño, J.P. Estudio de La Retrogradación En Películas Flexibles Obtenidas a Partir de Mezclas de Almidón Nativo de Yuca, Ácido Poli-Láctico (PLA) y Policaprolactona (PCL). Master’s Thesis, Universidad del Valle, Cali, Colombia, 2012. [Google Scholar]
Figure 1. Process for obtaining plantain flour and starch. (a) Obtaining flour; (b) obtaining starch.
Figure 1. Process for obtaining plantain flour and starch. (a) Obtaining flour; (b) obtaining starch.
Polysaccharides 06 00034 g001
Figure 2. Micrographs of flours and starches.
Figure 2. Micrographs of flours and starches.
Polysaccharides 06 00034 g002
Figure 3. FTIR spectra of plantain flours and starches.
Figure 3. FTIR spectra of plantain flours and starches.
Polysaccharides 06 00034 g003
Figure 4. X-ray diffractograms of plantain starches and plantain flours.
Figure 4. X-ray diffractograms of plantain starches and plantain flours.
Polysaccharides 06 00034 g004
Figure 5. Paste curves of native starches from plantain pulp and peel.
Figure 5. Paste curves of native starches from plantain pulp and peel.
Polysaccharides 06 00034 g005
Table 1. Plantain flour and starch samples.
Table 1. Plantain flour and starch samples.
CodeOriginPlantain By-Product
HPCACaucaPulp flour
APCAPulp starch
HCPCAPeel flour
ACPCAPeel starch
HPRRisaraldaPulp flour
APRPulp starch
HCPRPeel flour
ACPRPeel starch
Table 2. Characteristics of plantain peel and pulp by-products. Significance identification for homogeneous subsets (a, b) among the two origin treatments.
Table 2. Characteristics of plantain peel and pulp by-products. Significance identification for homogeneous subsets (a, b) among the two origin treatments.
SpeciesSourceBy-ProductDry Matter (%)Pulp/Peel RatioAverage Finger Weight (g)Average Diameter (cm)
Plantain (finger)RisaraldaPulp24.81 ± 1.71 a56.71 ± 3.95 a302.49 ± 27.23 a4.79 ± 0.47 a
Peel4.25 ± 2.96 b43.28 ± 3.95 b
CaucaPulp26.19 ± 3.03 a58.69 ± 2.37 a331.22 ± 33.37 a4.46 ± 0.33 a
Peel5.96 ± 2.01 b41.31 ± 2.37 b
Table 3. Influence of sodium metabisulfite concentration on starch extraction efficiency. Significance identification for homogeneous subsets (a, b) among the sodium metabisulfite content treatments.
Table 3. Influence of sodium metabisulfite concentration on starch extraction efficiency. Significance identification for homogeneous subsets (a, b) among the sodium metabisulfite content treatments.
TreatmentSodium Metabisulfite Content (%)Solution pHStarch Extraction on Dry Basis
(%)
Starch Extraction on Wet Basis
(%)
106.00 ± 0.0474.24 ± 5.89 a,b17.07 ± 1.35 a,b
20.15.94 ± 0.0472.47 ± 3.86 a16.67 ± 0.89 a
30.35.80 ± 0.0281.40 ± 1.28 b18.72 ± 0.29 b
40.65.71 ± 0.0678.05 ± 0.84 a,b17.95 ± 0.19 a,b
50.95.54 ± 0.0775.32 ± 2.52 a,b17.32 ± 0.58 a,b
61.25.46 ± 0.0480.21 ± 1.61 a,b18.45 ± 0.37 a,b
Table 4. Starch extraction yield from pulp by origin and sodium metabisulfite concentration. Significance identification for homogeneous subsets (a, b) among the plantain origin treatments.
Table 4. Starch extraction yield from pulp by origin and sodium metabisulfite concentration. Significance identification for homogeneous subsets (a, b) among the plantain origin treatments.
OriginSodium Metabisulfite Concentration
(%)
Starch Extraction on Dry Basis
(%)
Starch Extraction on Wet Basis
(%)
Cauca (APCA)0.376.70 ± 3.43 a19.03 ± 1.20 a
1.285.57 ± 2.51 b21.23 ± 0.62 b
Risaralda (APR)0.383.67 ± 0.12 b20.76 ± 0.03 b
1.289.81 ± 3.09 b22.28 ± 0.77 b
Table 5. Physical, physicochemical, thermal, techno-functional, and rheological properties of plantain’s flours and starches. Significance identification for homogeneous subsets (a–d) among the plantain origin treatments.
Table 5. Physical, physicochemical, thermal, techno-functional, and rheological properties of plantain’s flours and starches. Significance identification for homogeneous subsets (a–d) among the plantain origin treatments.
PropertiesPlantain Origin
CaucaRisaralda
PulpPeelPulpPeel
FlourStarchFlourStarchFlourStarchFlourStarch
CodeHPCAAPCAHCPCAACPCAHPRAPRHCPRACPR
Moisture (%)7.277.07-8.217.958.19-8.22
Ashes (%)12.59<2.0-12.0213.59<2.0-15.18
Crude fiber (% d.b.)49.6550.69-48.2043.8237.29-46.36
Protein (% d.b.)2.57<2.0-<2.02.60<2.0-<2.0
Lipids (% d.b.)<5.0<5.0-<5.0<5.0<5.0-<5.0
pH6.01 ± 0.05 d5.36 ± 0.09 c5.03 ± 0.03 b5.83 ± 0.06 d5.85 ± 0.13 d4.62 ± 0.02 a4.91 ± 0.01 b4.85 ± 0.05 b
Average diameter (µm)42.2031.42-32.5853.1633.40-49.06
Diameter–Wide (µm)-13.52 ± 5.21 c-9.80 ± 4.19 a-14.13 ± 4.66 c-12.00 ± 4.92 b
Diameter–Large (µm)-22.90 ± 8.16 b-18.26 ± 8.65 a-23.96 ± 8.26 b-22.88 ± 10.21 b
Amylose (%)-28.37 ± 0.28 c-18.6 ± 0.73 a-22.66 ± 1.59 b-17.76 ± 0.19 a
Crystallinity patternCC-BBB-B
Relative crystallinity (%)43.6745.78-37.0250.7746.09-33.39
Tm (°C)127.60125.51-125.93124.51122.67-122.82
ΔHm (J/g)92.1097.49-94.7189.0093.76-91.77
Td (°C)286.64311.03-290.60294.46316.92-303.71
WAI (g/g)-240.0 ± 1.0 a-328.0 ± 7.0 b-497.0 ± 56.0 c-444.0 ± 16.0 c
WSI (g/g)-91.0 ± 8.0 a-370.0 ± 10.0 d-122.0 ± 9.0 b-282.0 ± 17.0 c
SWP (g/g)-241.0 ± 1.0 a-334.0 ± 5.0 b-500 ± 46.0 c-450.0 ± 5.0 c
Onset temperature (°C)-73.00-71.60-66.80-63.90
Temperature pasting (°C)-86.50-91.60-90.90-90.60
Peak viscosity (Pa.s)-8.76-4.39-7.31-6.11
Breakdown viscosity (Pa.s)-5.32-3.62-4.40-4.64
Setback viscosity (Pa.s)-11.22-6.17-11.06-8.29
Disclaimer/Publisher’s Note: The statements, opinions and data contained in all publications are solely those of the individual author(s) and contributor(s) and not of MDPI and/or the editor(s). MDPI and/or the editor(s) disclaim responsibility for any injury to people or property resulting from any ideas, methods, instructions or products referred to in the content.

Share and Cite

MDPI and ACS Style

Castañeda-Niño, J.P.; Mina-Hernández, J.H.; Solanilla-Duque, J.F. Extraction and Characterization of Starches from the Pulp and Peel of Native Plantain (Musa AAB Simmonds) from Two Colombian Departments. Polysaccharides 2025, 6, 34. https://doi.org/10.3390/polysaccharides6020034

AMA Style

Castañeda-Niño JP, Mina-Hernández JH, Solanilla-Duque JF. Extraction and Characterization of Starches from the Pulp and Peel of Native Plantain (Musa AAB Simmonds) from Two Colombian Departments. Polysaccharides. 2025; 6(2):34. https://doi.org/10.3390/polysaccharides6020034

Chicago/Turabian Style

Castañeda-Niño, Juan Pablo, José Herminsul Mina-Hernández, and José Fernando Solanilla-Duque. 2025. "Extraction and Characterization of Starches from the Pulp and Peel of Native Plantain (Musa AAB Simmonds) from Two Colombian Departments" Polysaccharides 6, no. 2: 34. https://doi.org/10.3390/polysaccharides6020034

APA Style

Castañeda-Niño, J. P., Mina-Hernández, J. H., & Solanilla-Duque, J. F. (2025). Extraction and Characterization of Starches from the Pulp and Peel of Native Plantain (Musa AAB Simmonds) from Two Colombian Departments. Polysaccharides, 6(2), 34. https://doi.org/10.3390/polysaccharides6020034

Article Metrics

Back to TopTop