SJA_41_4_1604-1615

Introduction

The increasing global focus on environmental sustainability has driven a shift towards the development of environmentally friendly packaging materials. Edible films made from starch have emerged as a sustainable substitute for conventional plastic packaging. Starch, which is plentiful in a range of plant sources, is considered to have the ability to be biodegradable, renewable, and able to form films, making it the main ingredient in edible film production (Dick et al., 2015; Gadhave et al., 2018; Kumar and Neeraj, 2019; Jayarathna et al., 2022). Banggai yam starch, native to Indonesia, is known for its high starch content and is potentially underutilized (Cerqueira et al., 2011; Kusnandar et al., 2021; Ulyarti et al., 2021; Ambarwati et al., 2022; Chaniago et al., 2022). Starch phosphorylation, a chemical modification technique, increases its hydrophilicity, film-forming ability, and mechanical strength, thereby enhancing its function in film applications (Farahnaky et al., 2013; Ramadan and Sitohy, 2020; Malik et al., 2023).

Starch phosphorylation is a chemical modification technique that introduces phosphate groups into starch molecules that influence mechanical strength (Bruni et al., 2018; Wu et al., 2022; Gałkowska et al., 2023), increasing hydrophilicity (Liu et al., 2022; You et al., 2020), and film forming ability (Wang et al., 2018). This modification improves the compatibility of starch with plasticizers such as glycerol, which is added to increase film flexibility and reduce brittleness. However, the glycerol concentration plays an important role in determining the overall film properties, including tensile strength, elongation, and water vapor transmission rate (WVTR).

One plasticizer that is frequently used in food films is glycerol, which can have an impact on tensile strength, elongation, and water vapor transmission rate (WVTR) (Hamzah et al., 2021). The concentration of glycerol is very important in determining the overall properties of the film (Khotsaeng et al., 2023), maintaining the balance of mechanical resistance (Abou-Saleh et al., 2019; Ballesteros-Mártinez et al., 2020; Loo and Sarbon, 2020) and functional performance. Researching how the concentration of glycerol affects the mechanical and functional characteristics of phosphorylated Banggai yam starch food films is crucial to the creation of environmentally friendly packaging materials that perform better (Affandi et al., 2023).

This research aims to determine the effect of glycerol concentration on mechanical properties (tensile strength, elongation) and functional properties (WVTR, water and oil holding capacity, water content, biodegradability). By integrating recent advances and focusing on the specific properties of phosphorylated Banggai yam starch films, the research seeks to fill the knowledge gap regarding the optimization of glycerol content to maximize film performance.

Materials and Methods

The materials used in making phosphorylated Banggai yam starch include natural Banggai sweet potato starch, distilled water, 3% NaOH, Sodium Trimetaphosphate (STMP), Sodium Tripolyphosphate (STPP), HCl, and 95% ethanol. Meanwhile, the materials used in making phosphorylated Banggai yam starch edible film include Phosphorylated Banggai yam starch and glycerol.

Synthesis of edible film from phosphorized yam starch

Making edible films according to the method Abdul Rahim et al. (2011) with slight modifications. The main ingredient used Phosphate Banggai Yam Starch (PBYS) with the highest degree of substitution obtained from the results of the Phosphorylation stages of Banggai yam Starch carried out according to the method (Chaniago et al., 2023), which was previously modified using STMP 10%, STPP 2% and STMP/STPP ratio: 99/1 10%. The production of edible films involves preparing PBYS concentrations at four levels: 2.0, 3.0, 4.0, and 5.0 % (w/v) for each phosphorylation reagent. Glycerol 10, 30, 50% (w/v) of the weight of PBYS was added to this solution, then heated on a hot plate stirrer until it reached a temperature of 85oC and maintained for 11 minutes while continuing to stir. The solution is then poured into plates and dried in an oven at 50°C for 18-24 hours. The drying process is stopped after the edible film is easily removed from the plate. After drying, the film was cooled at room temperature for 15 minutes before being stored.

Mechanical characterization:

Stretch Strength or Tensile Strength: Stretching or tensile strength testing is a method for evaluating the mechanical strength of PBYS. The stretching strength of the edible film was measured using Lloyd's Universal Testing Instrument 50 Hz model 1000s using the ASTM D882-02 standard method, using (Rhim and Wang, 2013). The tensile strength at break is calculated by dividing the maximum force applied to the film until it tears (Newton) by the cross-sectional area of the film (mm2). Or mathematically it can be written as follows: Tensile strength = F/A

Information: F = tensile strength (N); A = cross-sectional area (mm2).

Elongation Percentage: Measurement of the elongation percentage provides information about the flexibility and elasticity of the PBYS. The percentage increase in maximum film length that occurs when a tensile force is applied until the film breaks about its beginning length is known as the elongation percentage. If the elongation percentage is less than 50%, it is considered good; if it is less than 10%, it is considered bad (Fardhyanti and Julianur, 2015). Here's the formula:

Percent elongation is classified as poor if it is less than 10% and as very good if it is more than 50%, under the Japanese Industrial Standard (1975) (Ariska and Suyatno, 2015).

Water Vapor Transmission Rate (WVTR): WVTR measurements help in evaluating PBYS's ability to control water vapor transfer, which is important in food packaging applications. WVTR is measured using the method suggested by (Xu et al., (2004). To create a saturated salt solution, a jar measuring 12 cm in diameter and 15 cm in height was used. The relative humidity (RH) was then adjusted to 75% by adding a 40% (w/v) room-temperature NaCl solution. Next, A 10 g silica gel was set in an acrylic cup with a diameter of 5 cm and a height of 1.8 cm. The cup was then covered with edible film that was proportional to its size and placed in a room with a relative humidity of 75%. The weight of the entire configuration was determined by weighing it every hour for 8 hours after water vapor was dispersed through the edible film and silica gel was added to the weight. The data is employed to generate a time-versus-time graph.

weight and slope are recorded to calculate WVTR using the following equation:

Functional characterization:

Water and Oil Holding Capacity (WHC and OHC): Measurement of water and oil holding capacity provides information about PBYS's ability to control water and oil content in food products. WHC and OHC are ascertained using a technique created by (Larrauri et al., 1996) with a few changes. In short, 250 mg of edible film samples were mixed with 25 mL of either olive oil or distilled water, shaken, and left to sit at room temperature for an hour. After centrifuging at 3,500 × g for 30 minutes, the residue was weighed and the water and oil holding capacities were calculated as g of water or oil per g of dried film edible sample, respectively (GS 150 Centrifuge, Clements, Sydney, Australia).

Water content

(AOAC, 1990) Water content analysis is an important parameter in understanding the stability and storage quality of PBYS.

Biodegradation properties:

Evaluation of the biodegradation properties of PBYS helps in understanding the environmental and sustainability impacts of this material. Each test specimen is first cleaned with sterile water for five minutes, then rinsed with 70% alcohol for five minutes. The specimen is then dried in a vacuum at 40°C for one night, weighed using an analytical scale, and finally buried in the soil. Test specimens were removed and cleaned every fifteen days, then they were rinsed with 70% alcohol, cleansed with sterile water, dried, and weighed once more using an analytical scale. Using weight tests, the rate of burial deterioration in this soil was determined (Nisah, 2018).

Results and Discussion

Mechanical characterization

PBYS Edible film strong-tensile

Tensile strength is the highest stretch a film can withstand before tearing or breaking. Determining the strength of the resulting film's ability to hold the material it is packaged in is the purpose of measuring tensile strength. The average combination value of PBYS weight treatment, phosphate reagent, and glycerol concentration on the tensile strength value of edible film can be seen in Figure 1.

Figure 1 shows that the average tensile strength values of PBYS edible films are different. The highest value in the B3R1P1 treatment (4g PBYS, 2% STPP, 10% Glycerol) was 31.88 MPa or N/mm2, the lowest value in the B2R2P3 treatment (3g, 10% STMP, 50% Glycerol) was 2.21MPa or N/mm2. This research shows that the greater the concentration of glycerol used, the tensile strength of edible film tends to decrease. According to Unsa and Paramastri (2010), lower tensile strength values can be caused by increasing the glycerol content, because it can reduce the energy required for molecules to move, resulting in a decrease in stiffness. In addition, decreasing intermolecular attractive interactions between adjacent polymer chains and reducing internal hydrogen bonds in molecules due to the addition of plasticizers can also reduce tensile strength (Putra et al., 2017; Uge et al., 2021). These results are also supported by research (Pradipta et al., 2020), that a higher plasticizer content can break hydrogen bonds in edible film thereby increasing flexibility. As a result, the resulting film will be more malleable, soft and flexible, causing its tensile strength to decrease.

Samples treated with glycerol have low or decreased tensile strength because glycerol is hydrophilic so it can accelerate the absorption of water vapor in the air and cause the film layer to break more quickly if pulled (Yanti, 2020). Glycerol can weaken the strength of polymer bonds (Anandito et al., 2012). The more glycerol added results in a decrease in tensile strength. This is caused by the chain bonds becoming stronger as a result of the increasing number of hydrogen interactions in the edible film so that to break the chain bonds a relatively large amount of energy is required (Haryani et al., 2022)

Percentage of elongation edible film PBYS

Elongation is the percentage elongation calculated when the film breaks during the drawing process. The percent elongation of starch-based edible films can be increased by adding plasticizers. The average value of the combination of heavy PBYS treatment, phosphate reagent, and glycerol concentration on the percentage value of elongation of edible film can be seen in Figure 2.

Figure 2 shows that the average percentage value of elongation for PBYS edible films is different. The highest value in the B4R2P3 treatment (5g PBYS, 10% STMP, 50% Glycerol) was 20.98%, and the lowest value was in the B1R2P1 treatment (2g PBYS, 10% STMP, 10% Glycerol) namely 1.30%. This shows that the addition of glycerol concentration can increase the elongation of PBYS edible film. Japanese Industrial Standards stipulate that good elongation ranges from 10-50%, and it is very good if it exceeds 50%. Therefore, some edible film samples are classified as having elongation that meets the standard (10.42-20.98%). According to Haryani et al., (2022) the elongation percentage rises as the glycerol content in the edible film increases. Next, follow the advice of Faizin et al., (2023) that a higher glycerol concentration will increase elongation since a higher elongation value is caused by an increased glycerol concentration. The results become more elastic with higher glycerol concentrations. Because edible film has a high flexibility value, it is easier to use when it has a high level of elasticity. The impact of elongation value results from a rise in glycerol concentration, which can weaken intermolecular interactions and enhance molecular chain mobility and edible film elongation (Putri et al., 2022).

Water vapor transmission rate (WVTR) Edible film PBYS

The amount of water vapor that permeates the surface of an edible film in a unit area and time is measured using a test called WVTR, or water vapor transfer rate. The thickness and surface shape of the edible film itself are factors that affect the pace at which water vapor diffuses. The film will have big holes and a relatively thin thickness the more water vapor permeates its surface (Ulyarti et al., 2021).

One of the characteristics of edible film that is used to calculate the material's permeability to water is the rate at which water vapor transmits. Glycerol, which is hydrophilic and often has a high degree of water vapor permeability, is a component of edible films. Figure 3 shows the average concentration value of the edible film's WVTR.

Figure 3 shows that the highest PBYS edible film water vapor transmission rate value was in the B3R1P3 treatment (4g PBYS, 2% STTP, 50% Glycerol), namely 1.59 g/m2 /hour, the lowest PBYS edible film vapor transmission rate value was in the B2R2P2 treatment (3g PBYS, STMP 10%, Glycerol 30%) namely 1.54 g/m2 /hour. The results of this research meet the JIS (Japanese Industrial Standard) (1975) standards, namely the maximum value is 10 g/m2/hour.

The more glycerol that is utilized, the faster the edible layer of water vapor spreads every hour. This is because glycerol is hydrophilic, or able to bind water. As a result, when the amount of hydrophilic components in the film increases, water vapor will be able to freely permeate the film, increasing the rate at which water vapor is transmitted (Alfatahillah et al., 2021). Conversely, the more glycerol utilized, the less water vapor transmission rate of edible film there is per hour. This is because sodium tripolyphosphate contains a phosphate group. Water has less opportunity to bind to starch because phosphate groups can link to the hydroxyl groups in starch (Ulfiasari et al., 2020). By binding to the hydroxyl group in starch, the phosphate group in sodium tripolyphosphate creates a cross-link that can stop water vapor from penetrating the substance. Additionally, straight chains of amylose produced by starch modification lead to the creation of cross-links between starch molecules, which reduces the hydrophilic qualities of the film. The water vapor transfer value decreases with increasing amylose content in starch films because amylose reduces its hydrophilic characteristics by forming a dense network. High amylose starch will make the film denser because of increased interactions between polymer molecular chains or the creation of cross-links, which will reduce the film's hydrophilic qualities (García et al., 2000).

Functional characterization

Determination of water holding capacity (WHC) and Oil (OHC) of edible film PBYS

The term "water holding capacity" (WHC) refers to a material's capability to hold water as well as its ability to bind water when introduced or during processing. WHC may be connected to the strength of water's attraction (Deden et al., 2020). The Water Holding Capacity (WHC) value of PBYS edible film can be seen in Figure 4.

Figure 4 shows that the average value of the water-holding capacity of PBYS edible film was the highest in the B3R1P1 treatment (4g PBYS, STPP 2%, Glycerol 10%) namely 0.34 g/g, and the average value of the water-holding capacity of PBYS edible film was the lowest in B3R3P1 treatment (4g PBYS, 10% STMP/STPP, 10% Glycerol) was 0.11 g/g. The results of this research show that It can be seen that there is a tendency to increase the water-holding capacity of PBYS edible film along with increasing glycerol concentration. This is by research (Anandito et al., 2012; Nugroho et al., 2013; Unsa and Paramastri, 2010). This is because glycerol dissolves readily in water and can raise the edible film's solubility percentage since it is hydrophilic, or it forms bonds with water. A decrease in the hydrophilic groups present in the constituent materials may lead to a reduction in the edible film's solubility (Waryoko et al., 2014). The high solubility of edible film demonstrates the hydrophilicity of the edible film as well as its decreased water resistance (Fardhyanti and Julianur, 2015). Hydrophilic (water soluble) and hydrophobic (oil soluble) components also have an impact on solubility. Glycerol and starch, which are hydrophilic substances and soluble in water, are used in this investigation (Zulferiyenni et al., 2014). The percentage of film solubility will rise when hydrophilic ingredients are added to edible film (Nugroho et al., 2013).

The concentration of glycerol as a plasticizer can affect the solubility of edible film in water. The solubility of starch-based films is dependent on the kind and quantity of plasticizer used. The solubility rises with the amount of plasticizers applied. Similarly, adding hydrophilic plasticizers to a mixture will make it more soluble in water (Coniwanti et al., 2015). According to Pangesti et al., (2014), the edible film's ability to hold water can be increased by the glycerol that has been added. Plasticizer glycerol has a low molecular weight, and a high boiling point, and is readily soluble in water. In addition, hydrophilic substances are included. More hydrophilic material will change the film's water solubility, increase the amount of dry material dissolved in water, and extend, add water, and relax the film structure, all of which will allow glycerol to increase the water distribution and WHC (Awwaly et al., 2010).

The resulting WHC value is also influenced by the fermentation process during modification (Dewi et al., 2022). The ratio of amylose to amylopectin, their molecular weights, the distribution of molecular weights, the degree of branching, and the length of the amylopectin molecule's outer branch, which may have an impact on the bonding group, are some of the factors that affect the WHC value, or water holding capacity (Aini et al., 2016).

The amount of oil that can be absorbed by the food ingredient's matrix is measured by its oil-holding capacity or OHC. OHC properties are used to measure a material's ability to retain the oil it absorbs (Giyarto et al., 2016). The Oil Holding Capacity (OHC) value of PBYS edible film can be seen in Figure 4. Figure 4 shows that increasing the glycerol concentration tends to reduce the oil-holding capacity of edible film. The highest average oil holding capacity value was in the B1R1P1 treatment (2g PBYS, 2% STPP, 10% Glycerol) namely 0.31 g/g, and the lowest average oil holding capacity value was in the B3R2P3 treatment (4g PBYS, 10% STMP, Glycerol 50%) is 0.12 g/g. The study's findings indicate that the oil-retaining capacity tends to diminish with increasing PBYS and glycerol concentrations. This is due to the Bengali tuber's starch granules' ability to draw in more water than oil. Using starch to create edible film can improve product integrity and shield goods from oxygen, carbon dioxide, and grease (Waryoko et al., 2014). Starch has a lipophilic part, this is shown by its ability to absorb oil. According to Rahim, et al., (2019) The proteins found on the surface of starch granules also affect oil absorption.

PBYS Edible film water content

When creating edible film, water content is crucial. Food will deteriorate more quickly the more water it contains. Edible films with lower water content characteristics are more popular as packaging for food products. This is because low water content can maintain the freshness and quality of food products for longer.

The water content of edible film is closely related to the transmission properties of water vapor. If the film has a low water content, the transmission of water vapor from the air to the food can be slower so that the product can be stored longer (Ali, et al., 2017). Edible film provides an important effect in maintaining water content because with edible film, water vapor in the environment is prevented from entering food products. If the film has a high water content, its ability to hold water vapor will be minimal (Yanti and Nairfana, 2023). The average water content value of edible film can be seen in Figure 5.

Water content has an impact on edible film's quality when it comes to storage or application as product packaging. The kind and quantity of components that go into making an edible film affect how much water it contains. The percentage difference between the material's pre- and post-heating weights can be used to calculate a material's water content. Based on Figure 5, it can be seen that the highest PBYS edible film water content value was in the B1R3P3 treatment (2g PBYS, 10% STMP/STTP, 50% Glycerol), namely 17.88%, the lowest PBYS edible film water content value was in the B2R2P1 treatment (3g PBYS, STMP 10%, glycerol 10%) which is 12.03%. This shows that the majority of research samples still meet the quality requirements for edible film. The quality requirement for edible film according to SNI 06-3735-1995 is to have a maximum water content of 16%. In addition, this research shows that the higher the glycerol concentration, the more likely it is to increase the water content of edible film. According to (Abdorreza et al., 2011), state that plasticizers can bind water. The edible film contains more water the more plasticizer is added. According to Amaliya and Putri, (2014) state that the number of solids will grow and the amount of water in the edible film will decrease with increasing polymer content in the film matrix. Both the fundamental ingredients and the components added during the film-making process affect how much water is in the edible film (Salimah et al., 2016).

Biodegradation properties of PBYS Edible film

Two factors that affect the biodegradation process are the kind of soil and the quantity of decomposing microorganisms present. The biodegradation of bioplastics is facilitated by around 90 different species of microorganisms, which include aerobes, anaerobes, photosynthetic bacteria, archaebacteria, and lower eukaryotes (Emadian et al., 2017). The biodegradation process of PBYS edible film in this study was carried out for 3 days, 6 days, and 9 days. The average graph of the PBYS edible film biodegradation process can be seen in Figure 6.

Based on Figure 6, it can be seen that the treatment of adding starch, different phosphate reagents, and glycerol concentration influences the biodegradation of PBYS edible film. With each increase in glycerol concentration, biodegradation tends to decrease as the added glycerol concentration increases. The highest biodegradation value for 3 days was found in the B1R1P2 treatment (2g PBYS, 2% STTP, 30% glycerol), namely 38.87%. The lowest biodegradation value for 3 days was in the B3R2P2 treatment (4g PBYS, 10% STMP, 30% glycerol), namely 20.27%. The highest biodegradation value for 6 days was found in the B2R1P2 treatment (3g PBYS, 2% STTP, 30% glycerol), namely 48.96%. Meanwhile, biodegradation for 6 days had the lowest value in the B3R2P1 treatment (4g PBYS, 10% STMP, 10% glycerol), namely 30.11%. Meanwhile, Biodegradation for 9 days had the highest value in the B1R1P2 treatment (3g PBYS, 2% STTP, 30% glycerol), namely 58.88%. Meanwhile, biodegradation for 9 days had the lowest value in the B1R2P3 treatment (2g PBYS, 10% STMP, 50% glycerol), namely 41.70%.

Edible films made with the addition of 30% glycerol concentration tend to experience a high or faster degradation process compared to edible films made with the addition of other glycerol. This research (Morina et al., 2023; Zulferiyenni et al., 2023) found that the amount of additional glycerol injected had an impact on how quickly the film deteriorated. High quantities of glycerol are added to the biodegradable film to make it stretchy and facilitate water absorption. As per Juliani et al. (2022), the biodegradable film's moisture content will rise due to glycerol's capacity to bind water. Because film wetness is a favorable environment for microbes, it is believed to be one of the variables that speed up the rate of biodegradation. The addition of glycerol can also accelerate the degradation of bioplastics because glycerol can absorb water easily (Lagos et al., 2015).

Conclusions and Recommendations

Research shows that glycerol concentration has a significant effect on the mechanical and functional properties of phosphorylated Banggai yam starch edible film. Increasing glycerol content increases film flexibility and water vapor permeability but reduces tensile strength and oil retention capacity. These findings highlight the importance of glycerol in balancing the mechanical integrity and functional performance of edible films, thereby contributing to the development of environmentally friendly packaging materials.

Acknowledgments

We want to thank the Ministry of Education, Culture, Research, and Technology of the Republic of Indonesia for funding this research so that it can run smoothly.

Novelty Statement

This study provides a comprehensive analysis of the mechanical and functional properties of phosphorylated Banggai yam starch edible films with varying glycerol concentrations, revealing that increased glycerol enhances film flexibility and water vapor transmission rate but decreases tensile strength and oil holding capacity. These insights are crucial for optimizing glycerol content to develop sustainable, high-performance packaging solutions.

Authors’ Contribution

Ramadhani Chaniago: Conceived and designed the research framework, supervised the experimental work, coordinated data interpretation, and prepared the initial and revised drafts of the manuscript

Asriani Hasanuddin: Supported the implementation of laboratory experiments, contributed to data acquisition, and assisted in interpreting functional and bioactive property analyses.

Abdul Rahim: Contributed to experimental design refinement, assisted in statistical analysis, and provided critical feedback to improve the scientific quality of the manuscript.

Darni Lamusu: Assisted in the preparation of native Banggai yam starch, contributed to laboratory procedures, and participated in manuscript editing.

Generative AI or AI assisted technology statement

The authors declare that no Generative AI was used in the creation of this manuscript.

Conflict of interest

The authors declare that there is no conflict of interest regarding the publication of this paper. This statement indicates that the authors have no financial or personal relationships that could inappropriately influence their work on this research study.

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