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IOP Conference Series:

Materials Science and


Engineering

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EXPOTECNOLOGIA 2020 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 1154 (2021) 012041 doi:10.1088/1757-899X/1154/1/012041

Synthesis of starch powder from different organic wastes: A


green approach to a valuable material

D P Sanabria1, H I Farfán1, D N Quintana1, I V Abril1, H F Castro1, R A


Paredes1, K L Roa1, 2
1
Universidad Pedagógica y Tecnológica de Colombia, Sogamoso, Colombia
2
Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada, Instituto
Politécnico Nacional, Ciudad de México, México

E-mail: [email protected]

Abstract. Plastic pollution has become one of the main causes of irreversible damages to the
environment. Despite the well-known adverse effects, the lack of culture in recycling is causing
overcrowded landfills with tons of this disposable material. Developing new products is
necessary to replace plastics with eco-friendly materials, in this way, biopolymers are a suitable
alternative. Biopolymer synthesis requires a natural polymer known as starch, which is a
common compound in roots, tubers, fruits, cereals and aquatic plants. In the present work, we
study different solid organic wastes such as cassava, potatoes, plantain, corn and two types of
algae Elodea Canadensis and Myriophyllum Quitense, in order to discover its feasibility as starch
sources. For this purpose, we established an extraction method taking into account the main
structure of each organic waste. By means of Fourier-transform infrared spectroscopy (FTIR)
and iodine test, we obtained the chemical structures and principal characteristics of each starch.
Synthesized powders exhibited characteristics of thermoplastic starches making them available
for its potential use in biopolymers.

1. Introduction
Plastics derived from petroleum have become necessary in several activities of human population
thanks to its benefits; however, its massive use is causing negative impacts to the earth. This
environmental problem has stimulated research to discover and propose new materials that can replace
plastics [1]. Accumulation of plastics rises up to 4900 millions of tons (almost 60% of total production)
in the atmosphere, according to current trends and dynamics of global waste management, by 2050
almost 9000 millions of tons will be recycled, 12000 millions of tons incinerated and 12000 millions of
tons left in landfills or in natural environments [2].
To develop eco-friendly alternatives to replace plastics is necessary to find a cheap, abundant and
renewable raw material; in this way, starch currently represents a widely used source for plastic
production with biodegradable properties. One natural source of starch is food; its wide consumption is
constantly creating high amounts of organic wastes that can potentially cause an environmental impact.
These organic wastes has an important content of starch that can be used [3]. Taking into account that
in Colombia, roots, fruits and tubers are involved within the food basket, a high consumption of these
could generate high amounts of organic husks. Nowadays the lack of recycling culture involve an
inadequate management of the organic wastes becoming sources of contamination [4].

Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distribution
of this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.
Published under licence by IOP Publishing Ltd 1
EXPOTECNOLOGIA 2020 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 1154 (2021) 012041 doi:10.1088/1757-899X/1154/1/012041

Another source of available starch that is causing significant environmental impacts is aquatic plants;
the principal cause is due to its endemic growth, which reduces the extension of lakes and lagoons. This
non-controlled growth cause decomposition, water quality alterations, poisoning of species and
ecological imbalance. Due to fertilizers used in the peripheral of the lacustrine body, algaes modified its
chemical composition causing a negative impact on other species [5].
One of the alternatives to mitigate these environmental problems are biopolymers, a class of
polymers made from renewable raw materials or derived from environment. These natural sources
makes them a sustainable option in terms of production. To develop natural polymers or biopolymers is
necessary a starch source. This polysaccharide is stored as energy reserve in plants; common starch
sources are roots (cassava), tubers (potatoes), aquatic plants (Elodea Canadensis and Myriophyllum
Quitense), fruits (plantain) and cereals (corn) [6].
Several works previously reported different extraction methods of starch, which include the wet or
traditional method. This method consisted of a solution of lactic acid and sulfur dioxide, which would
generate a change in the starch due to nixtamalization; a variation of the wet method is carried out with
the use of distilled water in other cases 25% sodium hydroxide [8] or buffer solutions [9] are used as
solvents. To accelerate the drying process and make an efficient separation, the centrifuge is usually
used [10], another procedure consist of decant for a long time suspending the material in water until the
sediment is obtained. Another existing method is through the dry route, in this procedure is necessary
to carry out repeated grinding, thus modifying the sugar content of the starch [11]. Currently, there are
methods whose purpose is to increase efficiency of extraction process using ultrasound-assisted
equipment. The method uses frozen roots, which has shown that 10 minutes of sonication promotes an
increase yield of starch. Additionally, it was shown that does not modify the structure of the starch
granule [12] making this method viable for the extraction of starch without changing the structure and
optimizing the yield.
In the present work, we investigate five different wastes as potential starch sources these include:
potato peels, cassava, plantain, corn (leaves and teas) and aquatic plants. To our knowledge, there are
reduced studies linked to starch extraction from the proposed wastes; therefore, findings of this work
are necessary and opening for further quantitative studies. Synthesis of starch carried out three phases;
in the first stage, we designed the extraction process, in the second we performed an iodine test for each
starch and last, we studied by means of Fourier-transform infrared spectroscopy (FTIR) each sample in
order to discover principal bands of chemical bonds formed. Finally, according to the extraction
efficiency we propose which organic wastes are potential starch sources to obtain biopolymers with
molecular balanced structures.

2. Materials and methods

2.1. Extraction process from organic wastes

Collected organic wastes used in this study such as corn husks, potato, plantain and cassava peels were
from different food companies located in Sogamoso, Colombia. The extraction process of starch was
designed based on the wet method [7] and is depicted in Figure 1. The process consisted of seven phases,
each one completed as follows:

- Selection: In this phase, we removed damaged and irregular peels from collected organic wastes.
- Washing: Organic wastes were subjected to three washes to remove impurities; first, raw materials
were cleaned carefully in a container with deionized water. Then, peels were disinfected
using 0.5% of hypochlorite mixed with 1000 mL of distilled water; solution was used per
1000 g of peels.
- Grinding: Raw materials were grinded using a disc mill to obtain a homogenous mass with less
polysaccharides.

2
EXPOTECNOLOGIA 2020 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 1154 (2021) 012041 doi:10.1088/1757-899X/1154/1/012041

- Filtration: 1000 g of mass was mixed with 1000 mL of deionized water was added and flocculated
for 2 hours to allow separation of starch granules from mass. Then, the mixture was passed
through a gauze filter to separate raw fiber from liquid. This process is repeated twice with
the dry matter remaining.
- Sedimentation: Filtered liquid was left at room temperature for 12 hours to allow accumulation of
starch particles. The sediment was washed using 200 mL of water per gram of starch, until
a clean material was obtained and finally decanted.
- Drying: The starch was dried at 40°C for 24 hours in an electric stove.
- Milling and sieving: Dry starch was passed through No. 40 sieve (400 microns).

Figure 1. Scheme of extraction process from wastes: corn husks, potato, plantain and cassava peels.

2.2. Extraction process from algaes

Two types of algaes were used Elodea Canadensis and Myriophyllum Quitense, both collected from
Lake Tota located in Boyacá, Colombia. As is showed in Figure 2 treatment of algaes and extraction
process of starch involved eight phases, described as follows:

- Washing: Aquatic plants were carefully cleaned with distilled water and disinfected with 0.5%
hypochlorite. Then, algaes were washed using 1000 mL of water per 1000 g of aquatic plants.
- Drying: Cleaned algaes were left on a surface and dried for 1 week at room temperature, avoiding
sun exposure.
- Crushing: Using an electric disk mill algaes were reduced to 400 microns.
- Filtration: 50 g of grinded aquatic plants were mixed with 700 mL of distilled water; the mixture
was flocculated for 2 hours to allow the release of starch particles. Then, the fiber was filtered
from liquid. This process was repeated twice with the remaining dry matter.
- Agitation: The mixture was stirred on a hotplate at 30 °C for 30 minutes and then filtered once.
- Sedimentation: The mixture was left for 24 hours to allow decantation of starch particles.
- Drying: Sediment was dried using a stove at 40 °C for 24 hours.
- Milling and sieving: Dried mass was milled to 400 microns using a mesh No. 40.

3
EXPOTECNOLOGIA 2020 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 1154 (2021) 012041 doi:10.1088/1757-899X/1154/1/012041

Figure 2. Scheme of extraction process from algaes Elodea Canadensis and Myriophylum Quitense.

The starch obtained of each sample was characterized through Fourier-transform infrared spectroscopy
(FTIR), for which the dry sample was mixed with KBr and pressed to obtain a tablet, which was
introduced in a Nicolet ™ iS50 FTIR spectrometer. For each of the samples, 32 scans were recorded in
the region of 400 to 4000 𝑐𝑚−1 [16].

3. Results & Discussion

3.1. Extraction efficiency

The amount of starch obtained in weight is shown in table 1 extraction efficiency obtained from potato
was 7.3%. Compared with an industrialized one with a yield of 15.56 to 17.76% [5] of starch from potato
residues, in this case, efficiency variation was affected by the extraction method used. The method was
carried out based on Gonzales L, Gómez S and Abad works, which were proposed as an effective
industrialized development. Based on works of Villalobos M, López P, Rodríguez and Prado M, the
extraction process is similar to the proposed in the present work and presented a starch content of
approximately 7 to 8 % [13]. The increase of efficiency in extraction of starch from potato peels, an
industrialized process is more convenient. In comparison with Bilgin work, starch extraction of plantain
peels has a higher starch efficiency reaching 11.3%. Works from Giraldo J, Cuarán J, García L, and
Pardo L, showed an efficiency of 12.3% [14]. The differences could be associated with quality of
plantain peels or differences in extraction processes. It should be noted that grain size could affected the
extraction efficiency of starch, since two solid phases remained once suspended water was removed.
Characteristic gray colour was observed as well, which could be characteristic of traces of proteins,
lipids and small starch granules. The last due to its low density which could not separate from water
remaining in white colour on surface [15]. The efficiency calculation was determined by equation (1),
determining the percentage efficiency (E) of each starch extracted from organic wastes and algaes:

𝑤𝑒𝑖𝑔ℎ𝑡 𝑓𝑟𝑜𝑚 𝑠𝑡𝑎𝑟𝑐ℎ 𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑒𝑑


𝐸= ∗ 100 (1)
𝑤𝑒𝑖𝑔ℎ𝑡 𝑠𝑎𝑚𝑝𝑙𝑒 𝑝𝑟𝑜𝑐𝑒𝑠𝑠𝑒𝑑

Table 1. Extraction efficiencies of potential starches as a percentage.


Type of starch % efficiency of obtaining
Potato 7,3
Plantain 6,7
Elodea Canadensis 4,15
Myriophyllum Quitense 3,82

4
EXPOTECNOLOGIA 2020 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 1154 (2021) 012041 doi:10.1088/1757-899X/1154/1/012041

3.2. Analysis of Fourier-transform infrared spectroscopy (FTIR)

The spectrum depicted in Figure 3 shows C-C elongation signals at 764 𝑐𝑚−1 , the signal 860 𝑐𝑚−1
allows displays a deformation of CH2; the range of 900 to 1250 𝑐𝑚−1 corresponds to the mostly
asymmetric stretching of the C-O bond vibrations, which are associated with the elongations of the
polysaccharide particles [17]. Besides, a decrease in the signals attributed to bending vibrations is
observed in 1243 𝑐𝑚−1 y 1650 𝑐𝑚−1. Also by elongation (3250-3900 𝑐𝑚−1) of the O-H groups; this
implies that the samples examined are hydrophilic. It is also noted that at 1344 𝑐𝑚−1 there is a
deformation of CH2.

Concerning the peak of the 1462 𝑐𝑚−1 which is why its deformation is evident. The signal at 2920
𝑐𝑚−1 corresponds to the C-H stretches of the glucose unit of the starch molecule; additionally, it was
observed that the 1740 𝑐𝑚−1 in each of the samples corresponds to the voltage vibration of C=O. The
results obtained showed considerable similarities with the typical band of a thermoplastic starch [18].
The links identified are shown in Table 2.

Table 2. Bonds resulting from Fourier-transform infrared spectroscopy.

Wavenumber Type of bond Description


(𝑐𝑚−1 )
3250-3900 O-H elongation Stretches related to intra and
Elongation CH intermolecular hydrogen bonds.
2920
1740 Elongation C=O
Bending (O-H)(Water) Hydroxyl groups confer
1650
hydrophilic properties.
1462 CH deformation or CH2
vibration

1344 C-O-H bending, CH2 vibration Characteristic bonds of


O-H bending crystalline starch/ amorphous
1243
starch region
1010, 1080, 1150 C-O and C-C Stretch

900 Elongation C-O Anhydroglucose units that are


860 Deformation CH2 stretched in the starch.
764 C-C elongation

According to the infrared transmission spectroscopy (Figure 4), the combinations of starches that
could be compatible for the manufacture of bioplastics are those that have flexions, elongations and
deformations (near wave numbers) in similar fragments, that is, they present chemical bonds related;
those mixtures were the potato-plantain, and corn-cassava [20].

5
EXPOTECNOLOGIA 2020 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 1154 (2021) 012041 doi:10.1088/1757-899X/1154/1/012041

Figure 3. FTIR of the starches studied (cassava, corn, potato, plantain, Myriophyllum Quitense and
Elodea Canadensis)

3.3. Iodine test

To verify starch structures in the organic material and algaes, the iodine test was performed [21]. The
procedure consist of adding 0.25 mL of iodine to a solution of 10 mL of distilled water with 1 g of
material to be tested. The reaction occurs when amylose is present, which has a non-branched helical
structure that allows the iodine to penetrate the helix of the starch, thus modifying the properties of light
absorption until obtain a blue color, although high concentrations displayed black color. As shown in
figure 4, after test was performed black color was displayed showing the presence of starch.

6
EXPOTECNOLOGIA 2020 IOP Publishing
IOP Conf. Series: Materials Science and Engineering 1154 (2021) 012041 doi:10.1088/1757-899X/1154/1/012041

Figure 4. Iodine test performed on Elodea Canadensis and Myriophyllum Quitense algaes.

4. Conclusions

Extraction efficiencies obtained showed that algaes used presented approximately 50% less starch than
organic peels, although the extraction process was carried out by the same method, and algaes were
subjected to an additional flocculation procedure using temperature.
The behavior found in starches extracted from potato, cassava and corn residues presented IR bands
that corresponded to typical structures of starch granules. Also, aquatic plants Elodea Canadensis and
Myriophyllum Quitense, possess the characteristics of the starch molecule, for this reason, it is possible,
in a next phase to give it a sustainable use as a biopolymer.
According to the FTIR analysis, starches have chemical functions similar to each other, because they
present the deformations, flexions and peaks on the same wavenumbers, therefore, the carbohydrates as
more similar bases for the elaboration of the bioplastics, were potato-plantain, and corn-cassava, varying
the quantities of the aquatic plants for the biopolymer.
The results of the iodine test applied to the material obtained from the aquatic plants showed a
positive result for the presence of starch, the most consistent coloration was in the Myriophyllum
Quitense concerning the Elodea Canadensis; which corroborates the existence of bonds associated with
the polysaccharide molecules detected by means of the analysis indicated by the infrared transmission
spectroscopy.

5. Future work

Based on the results obtained we recommend to characterized the fiber obtained as co-products from
the starch extraction process in order to take advantage of them for further applications.

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