Film Formulation Research Articles

Development of Edible Films Based on Nostoc and Modified Native Potato Starch and Their Physical, Mechanical, Thermal, and Microscopic Characterization.

Considering the potential of biopolymers from underutilized Andean sources in Peru to improve the characteristics of edible films, this work aimed to evaluate the formation of a polymeric matrix composed of Nostoc and modified potato starch for the formulation of edible films for food coating. The effects of polymer matrix ratio and drying temperature on films obtained by thermoforming were studied, determining the water vapor permeability and mechanical properties using a multifactorial design. Additionally, thermal properties were characterized by TGA and DSC, and structural properties by FT-IR and scanning electron microscopy. The results showed that the films exhibited lower solubility, lighter hues, better water vapor resistance, higher tensile strength, and improved thermal stability with increasing modified starch content. The formulation with higher Nostoc content exhibited a more homogeneous surface according to microscopy images, and no new chemical bonds were formed by adding modified starch and Nostoc to the polymer matrix, according to FT-IR spectra. These findings are promising and suggest using Nostoc for elaborating edible films composed of native and modified starch from native Andean potatoes as bio-based materials with potential application in the food industry.

Lignin and green solvent extracted phenolic compounds from date palm leaves as functional ingredients for the formulation of soy protein isolate biocomposite packaging materials: A circular packaging concept

The current study investigated valorization of lignin nanoparticles (LNPs) and phenolic compounds loaded in chitosan (DLECNPs) extracted from date palm leaves into the soy protein isolate (SPI) biocomposite films. The mechanical, structural, barrier, physiochemical, thermal, optical, antioxidant, and antimicrobial properties of the formulated composite films were investigated. The findings showed that the incorporation of DLECNPs into the SPI films significantly improved the film's antioxidant properties by more than 3 times and showed antibacterial inhibition zone in the range of 10–15 mm against six pathogenic bacteria. Further, incorporating LNPs into SPI-DLECNPs films notably improved the mechanical properties from 4.32 MPa and 29.27 % tensile strength and elongation at break, respectively to 10.13 MPa and 54.94 %, the water vapor permeability from 7.38 g/Pa s m to 5.59 g/Pa s m, and the antibacterial inhibition zone from a range of 10.2 mm to 15.0–21.5 mm as well as making the films more heterogeneous and stronger than control SPI film. Moreover, LNPs changed the initial films' color from light yellow to dark red and reduced the films' transparency. The results indicated that LNPs reinforced SPI composite films showed significant improvements in several properties and thus can be used as a potential ingredient for formulation of biodegradable packaging films.

Formulation and evaluation of bioadhesive buccal Films of Domperidone co-crystals by using Tamarind kernel powder as mucoadhesive polymer

As solubility plays key role in drug dissolution and bioavailability lots of techniques to enhance solubility are evolved. One of the techniques is co crystallization. The main aim of the work is to enhance the solubility of domperidone by co crystallization using coformers like Para amino benzoic acid and succinic acid. The cocrystals were evaluated for melting point and solubility enhancement. these cocrystals were used to prepare buccal films by solvent casting method. In the preparation of buccal films Tamarind kernel powder obtained from the seeds of Tamarind is used as mucoadhesive polymer and Hydroxy propyl methyl cellulose as film former, Polyethylene glycol 6000 as plasticizer, dehydrated banana powder as super disintegrant, sodium saccharin as sweetener and mixture of ethanol and water as solvents. The mucoadhesive strength of Tamarind kernel powder was determined using modified physical balance method. Four buccal films were prepared in which PDBF1 and PDBF2 are the two buccal films prepared using cocrystals of domperidone and Para amino benzoic acid and other two buccal films SDBF1 and SDBF2 with cocrystals of domperidone and Succinic acid. The buccal films were evaluated for different tests like folding endurance, swelling index and Surface pH. In vitro diffusion studies were conducted by Franz diffusion cell using egg membrane as semipermeable membrane and phosphate buffer of pH 7.4. The buccal films prepared with cocrystals of domperidone and succinic acid at weight ratio 1:2 has shown 86%drug release. The work has concluded that there is fold increase in aqueous solubility of Domperidone and the optimized formula is SDBF2 and Tamarind kernel powder can be used as mucoadhesive polymer in novel drug delivery systems. Keywords: co crystals, solvent evaporation, muco adhesive, buccal films, solvent evaporation

Biocompatible film based on protein/polysaccharides combination for food packaging applications: A comprehensive review

Protein and polysaccharides are the mostly used biopolymers for developing packaging film and their combination-based composite produced better quality film compared to their single counterpart. The combination of protein and polysaccharides are superior owing to the better physical properties like water resistance, mechanical and barrier properties of the film. The protein/polysaccharide-based composite film showed promising result in active and smart food packaging regime. This work discussed the recent advances on the different types of protein/polysaccharide combinations used for making bio-based sustainable packaging film formulation and further utilized in food packaging applications. The fabrication and properties of various protein/polysaccharide combination are comprehensively discussed. This review also presents the use of the multifunctional composite film in meat, fish, fruits, vegetables, milk products, and bakery products, etc. Developing composite is a promising approach to improve physical properties and practical applicability of packaging film. The low water resistance properties, mechanical performance, and barrier properties limit the real-time use of biopolymer-based packaging film. The combination of protein/polysaccharide can be one of the promising solutions to the biopolymer-based packaging and thus recently many works has been published which is suitable to preserve the shelf life of food as well trace the food spoilage during food storage.

Effect of the molar mass of chitosan and film casting solvents on the properties of chitosan films loaded with Mentha spicata essential oil for potential application as wound dressing

Chitosan based films endowed with antibacterial features have witnessed remarkable progress as potential wound dressings. The current study aimed at appraising the effects of the molar mass of chitosan (MM) and the film casting acids on the properties of unplasticized chitosan films and plasticized MSO-embedded chitosan films in order to provide best suited film formulation as a potential candidate for wound dressing application. The prepared films were functionally characterized in terms of their qualitative assessment, thickness, density, swelling behavior, water vapor barrier, mechanical and antibacterial properties. Overall, all chitosan films displayed thickness lower than the human dermis even though thicker and denser films were produced with lactic acid. Assessment of the swelling behavior revealed that only high molar mass (HMM) chitosan films may be regarded as absorbent dressings. Moreover, unplasticized HMM lactate (HMM-LA) films furnished lower stiffness and higher percent strain break as compared to acetate films, due to the plasticizing effect of the remaining lactic acid as alluded by the FTIR analysis. Meanwhile, they provided suitable level of moisture and indicated substantial antibacterial activity against S. aureus and E. coli, the most commonly opportunistic bacteria found in infected skin wound. Plasticized chitosan films doped with MSO were significantly thicker and more permeable to water compared to unplasticized films. Furthermore, MSO significantly potentiate the antibacterial effect of chitosan-based films. Therefore, plasticized HMM-LA/MSO chitosan film flashing good swelling behavior, adequate WVTR and WVP, suitable mechanical properties and antibacterial performances substantiated to be a promising antibacterial dressing material for moderately exuding wounds.

Fabrication of multifunctional ZnO@tannic acid nanoparticles embedded in chitosan and polyvinyl alcohol blend packaging film

The current study explores biodegradable packaging materials that have high food quality assurance, as food deterioration is mostly caused by UV degradation and oxidation, which can result in bad flavor and nutrition shortages. Thus, new multifunctional zinc oxide nanoparticles/tannic acid (ZnO@TA) with antioxidant and antibacterial activities were incorporated into polyvinyl alcohol/chitosan (PVA/CH) composite films with different ratios (1%, 3%, and 5% based on the total dry weight of the film) via a solution blending method in a neutral aqueous solution. Additionally, ZnO nanoparticles have unique antibacterial mechanisms through the generation of excessive reactive oxygen species (ROS) that may lead to intensify pathogen resistance to conventional antibacterial agents. Thus, minimizing the negative effects caused by excessive levels of ROS may be possible by developing unique, multifunctional ZnO nanoparticles with antioxidant potential via coordination bond between tannic acid and ZnO nanoparticles (ZnO@TA). ZnO@TA nanoparticles were examined using Fourier-transform infrared (FTIR), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The effect of the incorporation of ZnO@TA nanoparticles on the barrier, mechanical, thermal, antioxidant, antimicrobial, and UV blocking characteristics of chitosan/polyvinyl alcohol (ZnO@TA@CH/PVA) films was investigated. The lowest water vapor and oxygen permeability and the maximum antioxidant capacity% are 31.98 ± 1.68 g mm/m2 kPa day, 0.144 ± 5.03 × 10–2 c.c/m2.day, and 69.35 ± 1.6%, respectively, which are related to ZnO@TA(50)@CH/PVA. Furthermore, ZnO@TA(50)@CH/PVA film exhibits the maximum UV shielding capacity of UVB (99.994). ZnO@TA(50) @PVA/CH films displayed better tensile strength and Young`s modulus of 48.72 ± 0.23 MPa and 2163.46 ± 61.4 MPa, respectively, than the other film formulations. However, elongation % at break exhibited the most reduced value of 19.62 ± 2.3%. ZnO@TA@CH/PVA film exhibits the largest inhibition zones of 11 ± 1.0, 12.3 ± 0.57, and 13.6 ± 0.57 mm against Staphylococcus aureus, Aspergillus flavus, and Candida albicans, respectively. In accordance with these results, ZnO@TA@CH/PVA films could be utilized for food preservation for the long-term.

Evaluation of the introduction of buprenorphine-naloxone oro-adhesive film formulation to patients in NHS Lanarkshire

Evaluation of the introduction of buprenorphine-naloxone oro-adhesive film formulation to patients in NHS Lanarkshire

Malt bagasse in extruded wheat flour and PBAT biodegradable films

Malt bagasse (BM) is a byproduct of the brewing industry with low added value but is rich in fiber and proteins, making it a potential product to be incorporated into the formulation of biodegradable films. This work aimed to produce biodegradable films based on wheat flour and PBAT added with different concentrations of BM (0 – 7.5 %) by blown extrusion. The films were characterized by physical, optical, morphological, thermal properties, and compostability. It was possible to produce biodegradable films by blown extrusion with excellent processability. BM increased film opacity with a heterogeneous, rough, and yellowish surface. Also, BM addition in the films reduced their hydrophilicity; however, as the BM concentration increased, there was a reduction in the elongation at break, tensile strength, and thermal stability of the films. The film with 7.5 % BM showed greater fragmentation and mass loss during the composting process, possibly due to the fragile matrix that facilitated the action and degradation by microorganisms. The biodegradable films containing BM are viable alternative for packaging production for different products.

Optimizing film mechanical and water contact angle properties via PLA/starch/lecithin concentrations

The optimization of mechanical property and water contact angle of PLA/starch/lecithin film was conducted using response surface methodology. The tensile strength, Young's modulus and water contact angle of PLA/starch/lecithin film ranged from 0.44 ± 0.21–7.18 ± 0.57 MPa, 133.78 ± 33.7–775.57 ± 85.44 MPa and 17.71 ± 1.93–59.41 ± 28 (o), respectively. The amount of PLA and starch significantly impacts tensile strength and Young's modulus. Unlike starch, increasing PLA in the film formulation increases tensile strength and Young's modulus. The PLA-lecithin interaction decreases the film tensile strength and Young's modulus. The film water contact angle is statistically impacted by the PLA/starch interaction and quadratic term of lecithin. The adjusted R-square and p-value of each of the response ANOVA result indicates that the model quite captures the behavior of the responses. The response 2D plots also provide more insight into the variable behavior on the resulting response, making the response surface methodology a tool to design, develop and optimize PLA-based films.

Formulation and evaluation of amoxapine mucoadhesive buccal films

Among innovative drug delivery methods, buccal mucoadhesive systems have been attracting much interest recently because of their capacity to stick to the oral mucosa, stay there, and gradually release their drug content. By improving medication absorption through the oral mucosa and reducing the hepatic first-pass impact, buccal mucoadhesive films can increase the drug's bioavailability and enhance its therapeutic effect. The current study aimed to synthesize the medicine as a buccal bioadhesive film, which reduces the frequency of dosage form administration by releasing the drug at a sufficient concentration over time. Because this formulation is simple to administer and requires no water to swallow, improved patient compliance is one of its benefits. Dissolving profile as investigated in USP dissolving apparatus type 1 using saliva at pH 6.8. The impact of factors such as polymer type, concentration, and release profile of Amoxapine was investigated. The formulation was optimized Based on several evaluation criteria, including drug content and in-vitro drug release. Formulation F6 successfully releases the drug in 7 hours. The stability studies followed ICH recommendations, and the results showed that the optimized formulation was stable. The IR spectra demonstrated the stable qualities of Amoxapine in a mixture of polymers utilized and revealed the absence of interaction between the drug and the selected polymer.

Development and characterisation of agar/silver nanoparticles-based film from Gracilaria canaliculata for food packaging

Gracilaria canaliculata was used as a novel source to extract agar, and for the green synthesis of silver nanoparticles. Silver nanoparticles (0.1 - 0.3%) were incorporated into the agar matrix to develop an environment-friendly food packaging material using the solution casting method. The concentration of nanoparticles affected the physical, thermal, and mechanical properties of the films. Films containing higher concentrations of silver nanoparticles exhibited promising properties, and demonstrated strong antimicrobial activity against both Gram-negative and Gram-positive foodborne pathogens. The film formulation exhibited no cytotoxic effect on HepG2 cells, with cell viability exceeding 94%. These findings suggested that the film possessed favourable characteristics for use as a food packaging material, presenting a potential alternative to plastics.

Formulation and Characterization of Edible Film with Concentration Various of Sodium Carboxymethyl Cellulose from Kepok Banana (Musa paradisiaca L.) Bark and Plasticizer

Formulation and Characterization of Edible Film with Concentration Various of Sodium Carboxymethyl Cellulose from Kepok Banana (Musa paradisiaca L.) Bark and Plasticizer

Development of a Chitosan-Based Film from Shellfish Waste for the Preservation of Various Cheese Types during Storage.

The global concern about the use of disposable plastics has fed the research on sustainable packaging for food products. Among the virtuous materials, chitosan emerges as a valid alternative to conventional polyethylene films because of its abundance in nature. In this work, a novel film for food wrapping was developed by exploiting shellfish waste according to a vision of circular economy. Compared to previous studies, here, novel ingredients, such as polyvinyl alcohol (PVA), fibroin, and essential oils, were used in a synergistic combination to functionally postpone cheese deterioration. The fermentative procedure applied for the obtainment of chitin contributes to filling the existing gap in the literature, since the majority of studies are based on the chemical pathways that dramatically impact the environment. After pretreatment, the shrimp shell waste (SSW) was fermented through two bacterial strains, namely Lactobacillus plantarum and Bacillus subtilis. A deacetylation step in an alkaline environment transformed chitin into chitosan, yielding 78.88 g/kg SWW. Four different film formulations were prepared, all containing chitosan with other ingredients added in order of decreasing complexity from the A to D groups. The novel films were tested with regard to their physico-mechanical and antioxidant properties, including the tensile strength (12.10-23.25 MPa), the elongation at break (27.91-46.12%), the hardness (52-71 Shore A), the film thickness (308-309 μm), and the radical scavenging activity (16.11-76.56%). The performance as a cling film was tested on two groups of cheese samples: the control (CTR), wrapped in conventional polyethylene (PE) film; treated (TRT), wrapped in the chitofilm formulation deemed best for its mechanical properties. The volatiles entrapped into the headspace were investigated by means of the SPME-GC technique. The results varied across soft, Camembert, and semi-hard cheeses, indicating a growing abundance of volatiles during the conservation of cheese. The bacterial growth trends for mesophilic, enterobacteriaceae, and lactic acid bacteria were expressed as the mean colony forming units (CFU)/mL for each type of cheese at different sampling times (day 2, day 8, and day 22): the highest load was quantified as 8.2 × 106 CFU/mL at day 22 in the CTR Camembert cheese. The TRT samples generally exhibited inhibitory activity comparable to or lower than that observed in the CTR samples. The sensory analysis revealed distinctions in cheese taste between the TRT and CTR groups.

Plasticulture film coextruded with essential oils: sustainable protection of salad crops

ABSTRACT Plasticulture has revolutionised Farming production. In salad cultivation, the snail is the main pest that can cause significant economic losses. The present study focuses on the design of a new industrial mulching material co-extruded separately with three essential oils: cade, turmeric and cumin oil. Experimental tests carried out on a pilot system confirmed the repellent effect against this mollusc and the protection of lettuce weight loss by about 30%. Adhesion tests by Escherichia coli and Pseudomonas aeruginosa demonstrate anti-adhesion properties of 80% when bioactive oils are incorporated into the industrial formulation of the plastic film. Application of the predictive theoretical approach confirms that the adhesion scores cannot be explained by the total adhesion energy and total hydrophobicity energy. This proves that these effects are the result of bioactive activity. This research work offers an innovative, practical and ecologically responsible alternative to protect lettuce crops against nuisances and pests.

Indicator Films Containing Dendrobium Orchid Flower Extract and TiO2 Nanoparticles for Monitoring Fish Fillet Spoilage

This work aimed to study a novel pH indicator film prepared from carboxymethyl cellulose (CMC)/tapioca starch (TS) incorporating Dendrobium orchid flowers and TiO2 nanoparticles for monitoring fish fillet freshness. The films were prepared based on carboxymethyl cellulose (CMC) and tapioca starch (TS) blend (CMC/TS) incorporated with TiO2 nanoparticles and Dendrobium orchid flower (DOF) extract. The result showed that the DOF extract contained peonidin-3,5-O-diglucoside and exhibited distinguishable color changes in different pH buffers. Likewise, the CMC/TS+TiO2+DOF film’s color changed corresponding to the extract. The X-ray diffraction analysis revealed the expansion of the film’s amorphous region, due to the intermolecular interactions. Analyzing scanning electron microscope images showed the effects of TiO2 and DOF extract on the surface morphology of films. The incorporation of TiO2 and DOF extract into the film formulation improved various film properties, such as redness, opacity, tensile strength, and water solubility. For the sensitivity testing, the color of the CMC/TS+TiO2+DOF film responded to ammonia vapor more than acetic acid vapor, suitable for monitoring seafood spoilage behavior. In addition, the application of film for monitoring the freshness of fish fillets was conducted. The CMC/TS+TiO2+DOF film color changed from purple to bluish-purple corresponding to the spoilage of samples. Indicating its potential as an indicator for monitoring fish fillets' freshness.

Synthesis of cellulose nano fiber from palmyrah fruit fiber and its applicability as a reinforcement agent on starch based biodegradable film

The global trend in packaging is shifting towards environmentally friendly, natural materials that decompose easily. Among the bio-based packaging materials, starch is a renewable, biodegradable, bio-compatible, and easily accessible source. However, starch-based biodegradable films depict weak mechanical properties compared with synthetic polymers. This problem can be solved by incorporating reinforcement fillers into the starch matrix. Palmyrah fruit (Borassus flabellifer L.) waste can be a good source to obtain fillers due to its high cellulose content. The aim of the study was to investigate the reinforcement of starch-based biodegradable films with the incorporation of pure cellulose nanofiber (CNF) obtained from palmyrah fruit fiber (PFF). Chemical treatments such as alkaline treatment (4% NaOH), bleaching [1% Ca(OCl)2], and acid hydrolysis (10 moldm-3 H2SO4) were done successively to obtain pure CNF from PFF. CNF was characterized using FTIR and particle size distribution (PSD) was analyzed by granulometry. The yield of CNF from PFF was 37.890±0.008 %. The results of FTIR depicted CNF was synthesized successfully. Five different biodegradable films were prepared by varying the amount of palmyrah tuber starch (4.5-2.5 w/w %) and CNF (0.0-2.0 w/w %) while the amount of glycerin (1.5 w/w %) and gelatin (1 w/w %) were kept constant. PSD results revealed that nano-sized CNF (10-100 nm) was synthesized successfully. The optimized film was selected based on the tensile strength and low water vapor transmission rate. Optimized film formulation, with palmyra tuber starch (3 w/w %) and CNF (1.5 w/w %) showed desirable physical, mechanical and optical properties, including the thickness, moisture content, water vapor transmission rate, water uptake, transparency at 600 nm, water activity, water solubility and tensile strength of 0.192±0.004 mm, 11.07±0.04 %, 3.870±0.005 g/m2.day, 22.34±0.05 %, 3.97±0.01 %, 0.440±0.001, 51.68±0.140 % and 9.55 MPa respectively. All films showed excellent soil biodegradability within two weeks. In conclusion, palmyra fruit CNF can be effectively used to reinforce starch-based biodegradable packaging films.

A microfluidic platform for automatic continuous flow layer‐by‐layer assembly of polymer multilayered nanofilms

AbstractCapillary flow layer‐by‐layer assembly is a microfluidic platform for high throughput preparation and screening of multilayered polymer nanofilms. However, it is time‐consuming and labor‐intensive, since the switching of polyelectrolyte solutions is done manually. As the emergence of flow chemistry and microdevices for artificial intelligence‐based lab automation, an automatic system that can switch polymer solutions and washing liquids is urgently needed for building functional LbL films inside microfluidic devices. Herein, we construct a continuous flow (ConF)‐layer‐by‐layer (LbL) device that can automatically fabricate polymer nanofilms inside a microfluidic device. By including a flow separator and a mixer (a model polyelectrolyte pair), chitosan and carboxymethyl cellulose can be deposited inside a microfluidic device using the ConF‐LbL system. Resulting nanofilms are studied by investigating thickness and surface roughness of the nanofilms and comparing with the other conventional LbL methods. The acid dissolution method was used to compare the differences in stability between nanofilms made from ConF‐LbL and static immersive method in similar conditions. Furthermore, by using one optimized film formulation for coating on the inside walls of a microfluidic chip, we successfully demonstrated the ability of this device to capture cancer cells in whole blood. This ConF‐LbL platform is expected to be a convenient tool to coat functional nanofilms inside microdevices for biomedical and sensor applications.

Recent progress in polyvinyl alcohol (PVA)/nanocellulose composite films for packaging applications: A comprehensive review of the impact on physico‐mechanical properties

AbstractAs society advances, the demand for innovative and sustainable food processing techniques and materials has grown significantly. The food industry, especially the food packaging sector, faces the challenge of developing cost‐effective and sustainable packaging materials to meet consumers' increasing demands. One promising solution for this is the use of biodegradable polymers such as polyvinyl alcohol (PVA), but standalone PVA cannot meet the required properties of packaging materials. The use of nanocellulose (NC) as fillers has been intensively studied recently. This review article provides a comprehensive overview of existing studies focusing on the preparation of PVA/NC composite films for packaging applications. The effects of NC loading on the physico‐mechanical properties of these films, including tensile strength, elongation, water absorption/swelling behavior, barrier properties, and optical properties, have been thoroughly examined. Overall, the general findings suggest that the reinforcement of NC in the PVA polymer matrix leads to improvements in the films' properties. Specifically, the addition of NC enhances tensile strength, reduces O2, CO2, and water vapor transmission rates, and decreases the films' propensity to absorb moisture or swell under wet conditions. However, it is important to note that the presence of NC compromises the optical properties of the films by reducing transparency, and the NC content beyond threshold level reduces the feasibility of the composite film. By synthesizing these findings, this review underscores the potential of PVA/NC composite films as promising materials for packaging applications. Moving forward, further research efforts are warranted to optimize the formulation and processing of these composite films to strike a balance between mechanical strength and optical clarity, thus advancing their practical utility in the packaging industry.

Developing a synergistic rate-retarding polymeric implant for controlling monoclonal antibody delivery in minimally invasive glaucoma surgery

Monoclonal antibodies (mAbs) have garnered substantial attention within the field of ophthalmology and can be used to suppress scar formation after minimally invasive glaucoma surgeries. Here, by controlling mAb passive diffusion, we developed a polymeric, rate-controlling membrane reservoir loaded with poly(lactic-co-glycolic acid) microspheres to deliver mAb for several weeks. Different parameters were tested to ensure that the microspheres achieved a good quality characteristic, and our results showed that 1 %W/V emulsifier with 5 %W/V NaCl achieved mAb-loaded microspheres with the highest stability, encapsulation efficiency and minimal burst release. Then, we fabricated and compared 10 types of microporous films based on polylactic acid (PLA), polycaprolactone (PCL), and polyethylene glycol (PEG). Our results revealed distinct pore characteristics and degradation patterns in different films due to varying polymer properties, and all the polymeric film formulations showed good biocompatibility in both human trabecular meshwork cells and human conjunctival fibroblasts. Finally, the optimized microspheres were loaded into the reservoir-type polymeric implant assembled by microporous membranes with different surface coating modifications. The implant formulation, which was fabricated by 60 PCL: 40 PEG (3 %W/V) polymer with 0.1 %W/V poly(lactic-co-glycolic acid) barrier, exerted the best drug release profile that can sustained release mAb (83.6 %) for 4 weeks.

Antimicrobial Solid Starch-Iodine Complex via Reactive Extrusion and Its Application in PLA-PBAT Blown Films.

In this study, a solid masterbatch of starch-iodine complex with 6.7 wt.% iodine was prepared in pellet form using a ZSK-30 twin-screw extruder. Thermogravimetric (TGA) and isothermal TGA analysis of the pellets revealed that there was no significant loss of iodine due to sublimation during reactive extrusion. These solid pellets demonstrated antifungal properties when applied to strawberries via dip coating in an aqueous solution, extending their shelf life from two days to eight days, thereby reducing fungal growth and visual decay. Furthermore, the solid pellets displayed antibacterial activity against E. coli, as evidenced by the clear zone of inhibition observed in the Kirby-Bauer test. To enhance practical application, these pellets were further blended with PLA-PBAT film formulations at 10 and 18% by wt. to make blown films with effective iodine loadings of 0.7 and 1.3% by wt. These films showed superior antibacterial activity against E. coli compared with PLA control films and the commercial silver antimicrobial-containing films during direct inoculation tests as per ISO 22196. Tensile strength and elongation at break in machine direction (MD) for the starch-iodine-containing blown films were comparable to the control films in MD, but tensile strength was reduced to 37-40% in the transverse direction (TD). This was due to a non-uniform dispersion of the starch-iodine complex in the films, as confirmed by the visual and SEM analyses. Thus, this study illustrates the practical utility of the solid starch-iodine complex as a safe and efficient means of introducing iodine into an environment, mitigating the typical hazards associated with handling solid iodine.