Production of Antioxidant Black Rice-Polyurethane Biocomposite as Food Packaging and Wound Healing Product
1. Introduction
Wound dressings are medical textile products that help wounds heal rapidly in health-friendly environments and conditions (Ersoy et al., 2015). Medical textiles, or so-called medtech textile materials, have been developing rapidly in the textile industry recently. Medical textiles are textile materials produced or designed for medical applications. Surgical yarns, dressings, bandages, artificial organs and similar materials are classified as medical textile products (Dogan and Basal, 2009). Medical textiles are textile materials designed for widespread use in all areas of medicine and surgery.Medical textiles should be biocompatible with surrounding tissues and should be combined with different materials. The general characteristics desired from medical textiles depending on the field of use include: strength, non-toxicity, elasticity, hypoallergenicity, durability and biocompatibility.
Biomedical materials can be contaminated with bacteria, and sterilization of biomedical materials is one of the most important elements (Al-sherbini et al., 2015). Antioxidants have become one of the important issues in human nutrition in recent years, due to the ability of free radicals to cause damage. In addition, synthetic and natural antioxidants have been used as nutrient treatments for a long time. While these antioxidants protect food, they also demonstrate protection against oxidizing substances (Yavaşer, 2011). Antioxidants strengthen the body's immune system and possess properties such as anti-aging effects.Black rice is a nutrient source with high antioxidant value. The aroma of black rice derives from acetyl pyrrole, while its color derives from anthocyanin, cyanidin and 3-O-beta glucoside (Shao et al., 2018).
Polyurethanes (PU) are copolymers containing urethane groups in their structures (Yeganeh and Hojati-Talemi, 2007). Their physical and mechanical properties and good biocompatibility have provided a wide variety of applications (Gültekin, 2006). With these properties, polyurethane is also used as a wound dressing material. Wound dressing facilitates epidermal cell migration by preventing water loss from the wound surface (Zlatanic et al., 2004). Figure 1 shows the linear PU structure.Figure 1. Linear PU structure (Zlatanic et al., 2004)
In this study, food packaging products and wound healing tape materials were produced from PU-black rice biocomposites using the electrospinning method. Characterization studies of nanostructured composites were conducted using structural (FTIR), morphological (FEGSEM), thermal (DSC) and mechanical (tensile) analysis. The prepared PU nanofiber structures with black rice additive are expected to have significant potential primarily as food packaging products and wound healing tape materials in tissue engineering.2. Materials and Methods
2.1 Materials Used
Black rice was obtained from a local market in Istanbul. In biocomposite production, PU (Lubrizol Advanced Material Inc. Cleveland United States) was used, and dimethylformamide (DMF-HCON(OH3)2) (Sigma-Aldrich/Turkey) and ethyl acetate (C4H8O2) (Sigma-Aldrich/Turkey) were used as organic solvents to dissolve the polymer. In the electrospinning phase, biocomposite was used as the collector material on oil-based paper.2.2 Production of Black Rice Reinforced PU Nanofibers by Electrospinning Method
14% PU nanofibers with the addition of 1%, 5%, and 8% black rice were dissolved in a DMF/ethyl acetate solvent system mixed at 80/20% by volume at 40°C for 2 hours and made suitable for the nanofiber production process using the electrospinning method. The nanofiber production process was performed on 1%, 5%, and 8% black rice-reinforced 14% PU solutions and on the 14% PU matrix. The production process was based on the parameter values shown in Table 1. Table 1 displays the parameter values applied to the electrospinning solutions. Figure 2 shows the production stages of the biocomposite product.Table 1. Biocomposite production parameters by electrospinning method (Bozkurt et al., 2017)
Figure 2. Production of black rice reinforced PU nanofibers by electrospinning
2.3 Characterization Studies
For structural analysis of the biocomposites, the functional groups present in the sample structures were determined based on percent transmittance (T%) in the wavelength range of 400-4000 cm⁻¹ using a Jasco 6600 FTIR device. For morphological analysis, a Quanta FEG 450 FEGSEM device was used to obtain high-resolution nanofiber images, and the average diameter thickness of these nanofibers was measured using Image J (2011) software. For thermal analysis, a Hitachi 7000X instrument was used at 10°C/min heating rate.DSC analysis was applied to 10 mg weighed biocomposite samples in 3 steps over a temperature range of -50-140°C.
For mechanical analysis, according to ASTM standards, sample thickness was measured with an OKR brand micrometer for samples cut to 1x5 cm, and a Zwickline test device was adjusted to a tensile speed of 5 mm/minute under 500 N load to determine mechanical properties. In the test process, three replications were made from four different samples and their mean values were used as reference.3. Discussion 3.1 FTIR Analysis
When the PU structure spectrum was evaluated, it was determined that the N-H stretching band was at 3325 cm⁻¹, the CH₂ stretching band was at 2956 cm⁻¹, and the C=O absorption bands were at 1701 and 1727 cm⁻¹ wavelengths. The C-C stretching bands in the benzene ring had frequencies of 1464 cm⁻¹ and 1597 cm⁻¹, the N-H and C-N bond bands in the amide group had a wavelength of 1527 cm⁻¹, and the C-O-C stretching bands were at 916 cm⁻¹ and 1100 cm⁻¹ wavenumbers (Chiono et al., 2014). The black rice particles reduced the wavelength intensity of the PU structure's functional groups while simultaneously shifting the stretching band values slightly. In the 14% PU-8% black rice biocomposite structure, it was observed that the functional groups of PU and black rice particles overlapped. Figure 3 shows the FTIR spectrum of the PU-black rice biocomposite.Figure 3. FTIR spectrum of PU-black rice biocomposite
3.2 FEGSEM Analysis
It was found that black rice particles reinforced into the polymeric matrix reduced agglomeration formation as concentration increased. It was observed that as the concentration ratio of the reinforced black rice particles increased, the black rice particles were homogeneously coated on the fibers. In addition, during the electrospinning stage, it was determined that nanofiber dispersion varied depending on flow rate, voltage, distance between the collector plate and feeder tip, and collector plate rotation speed.The fiber structures of samples with increased concentration were determined by FEGSEM images showing homogeneous fiber shapes with no agglomeration as fibers thinned (Tijing et al., 2012; Bozkurt et al., 2017).
The nanofiber diameters were measured with Image J (2011) software using one of the FEGSEM images shown in Figure 4. The nanofiber diameters decreased with increasing black rice particle concentration. The nanofiber diameters ranged from 30-350 nm as measured with Image J (2011) software. Approximately 50 nanofiber structures were measured and their average diameter values were used as reference. Figure 4 shows the FEGSEM images of PU-black rice biocomposites.Figure 4. FEGSEM images of PU-black rice biocomposites
3.3 DSC Analysis
When the thermal analysis results of the PU-black rice biocomposite were examined, it was observed that the glass transition temperature (Tg) and melting point (Tm) increased with increasing black rice concentration in the black rice-reinforced biocomposites compared to pure PU polymer. Biocomposites with high thermal properties were obtained for use in food packaging and wound healing products (Anandhan and Lee, 2014). Figure 5 shows the DSC analysis results of PU-black rice biocomposites.3.4 Tensile Analysis
It was observed that the strength value increased linearly with increasing concentration percentages of black rice particles reinforced into the PU matrix material. As can be seen from the FEGSEM images obtained from morphological investigations, the mechanical properties of these biocomposites increased in accordance with results showing that black rice particles were homogeneously coated on polymer fibers with no agglomeration formation. Biocomposites were produced with strength values exceeding those found in comparable studies in the literature. The 14% PU-8% black rice sample yielded the highest strength value obtained in this study. It was concluded that this increase in strength resulted from the high load-bearing capacity of the polymeric matrix, the reinforcement by black rice particles, and their homogeneous distribution in the biocomposite (Bozkurt et al., 2017). Figure 6 shows the tensile test values graph of PU-black rice biocomposites.4. Conclusion
When the study results were evaluated, biocompatible and biodegradable food packaging products and wound healing tape were successfully produced from black rice-reinforced PU matrix materials. The functional groups determined by FTIR analysis and the black rice and PU materials contained in the PU-black rice biocomposite structure were identified. As a result of FEGSEM analysis, the fiber sizes of PU and PU-black rice nanofibers were determined to be 30-350 nm using Image J (2011) software. It was observed that the nanofiber diameters of these fine fibers remained intact, and black rice particles encircled the PU fibers homogeneously. When mechanical tests were applied to the produced biocomposites, the highest test value was reached with the 14% PU-8% black rice biocomposite compared to other samples. With additional tests such as antioxidant and cell culture studies, the biocomposite samples will be able to guide future research.Acknowledgment
We thank the Arel University ArelPOTKAM (Polymer Technologies and Composite Application and Research Center) team and the Zwick-Roell company managers and employees who assisted in the mechanical analysis studies of the biocomposites.- References ERSOY, Y., DURAN, M., & TAYYAR, A. E. (2015). Medical Textiles and Wound Dressing. Düzce University Science and Technology Journal, 3(2). DOGAN, G., & BASAL, G. (2009). Use of biopolymer nanofibers obtained by the electrospinning method as drug delivery systems, wound dressing and tissue scaffolds. Electronic Journal of Textile Technologies, 3(2), 58-70. AL-SHERBINI, A., RAGAB, S. S., & EL-SAYED, H. H. (2015). Antimicrobial Effects of Silver Nanoparticles Mediated Cosmetic Cream and Cotton Gauze on Candida Strains. Journal of Pharmacy and Biological Science, 10(3), 69-75. YAVAŞER, R. (2011). Comparison of the antioxidant capacity of natural and synthetic antioxidant compounds, Master's Thesis, Adnan Menderes University, Institute of Science, Aydın. SHAO, Y., Hu, Z., YU, Y., MOU, R., ZHU, Z., & BETA, T. (2018). Phenolic acids, anthocyanins, proanthocyanidins, antioxidant activity, minerals and their correlations in non-pigmented, red, and black rice. Food Chemistry, 239, 733-741. YEGANEH, H., & HOJATI-TALEMI, P. (2007). Preparation and properties of novel biodegradable polyurethane networks based on castor oil and poly (ethylene glycol). Polymer Degradation and Stability, 92(3), 480-489. GULTEKIN, G. (2006). Production of fatty acid-based polyurethane films for wound dressing material applications, Master's Thesis, Istanbul Technical University, Institute of Science, Istanbul. ZLATANIC, A., LAVA, C., ZHANG, W., & PETROVIC, Z. S. (2004). Effect of structure on properties of polyols and polyurethanes based on different vegetable oils. Journal of Polymer Science Part B: Polymer Physics, 42(5), 809-819. BOZKURT, Y., SAHIN, A., SUNULU, A., AYDOGDU, M. O., ALTUN, E., OKTAR, F. N., ... & GUNDUZ, O. (2017). Electrospun Nanocomposite Materials, A Novel Synergy of Polyurethane and Bovine Derived Hydroxyapatite. In Journal of Physics: Conference Series (Vol. 829, No. 1, p. 012015). IOP Publishing. CHIONO, V., MOZETIC, P., BOFFITO, M., SARTORI, S., GIOFFREDI, E., SILVESTRI, A., ... & DI MEGLIO, F. (2014). Polyurethane-based scaffolds for myocardial tissue engineering. Interface Focus, 4(1), 20130045. TIJING, L. D., RUELO, M. T. G., AMARJARGAL, A., PANT, H. R., PARK, C. H., KIM, D. W., & KIM, C. S. (2012). Antibacterial and superhydrophilic electrospun polyurethane nanocomposite fibers containing tourmaline nanoparticles. Chemical Engineering Journal, 197, 41-48. ANANDHAN, S., & LEE, H. S. (2014). Influence of organically modified clay mineral on domain structure and properties of segmented thermoplastic polyurethane elastomer. Journal of Elastomers & Plastics, 46(3), 217-232.
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