Fabrication and characterization of biopolymer/salicylic acid/algae/ZnO nanoparticle multi functional nanofiber materials

Nanofibers are materials which have high strength, flexibility and nanometer-sized fibers with high surface area. They can be synthesized from many different polymers, composed with inorganic materials and produced with different physical and chemical properties with the help of inorganic materials. Today, polymer nanofibers are used in a wide variety of applications. Studies on the use of nano fibers in biomedical and cosmetic fields have shown a great increase in recent years. A wide variety of natural polymers, synthetic polymers and combinations of them are frequently used in medical and biological applications. Recently, the use of natural polymers such as gelatin, collagen and silk fibroin and synthetic polymers like polyglycolic acid (PGA), poly (L-lactide) (PLA), poly (lactide-co-glycolide) (PLGA) and poly (ε-Caprolactone) (PCL) in nanofiber production by electrospinning method has increased. In addition, combinations of natural and synthetic polymers such as PCL / Gelatine and PLGA / Collagen are also used in the production of nanofibers by electrospinning. Although many different polymers and inorganic additives can be used in the production of nanofibers, the gelatin from natural polymers is widely preferred because of its biocompatibility properties and biodegradability in nature. PCL which is a synthetic polymer also has biocompatible and biodegradable properties. Gelatin/PCL composite nanofibers show better mechanical and characteristic properties than gelatin or PCL nanofibers alone. Furthermore, there is no need to crosslink the Gelatin/PCL composite nanofibers. Because they maintain the fiber diameter and porosity. Zinc oxide (ZnO) is a metal oxide used in the production of nanofibers. They used in biomedical and cosmetic applications due to its antibacterial and wound healing properties. Zinc oxide; due to its antibacterial, wound healing, anti-redness, anti-inflammatory etc. properties, it has the potential to be used in face masks used in cosmetics sector against acne problem. However, zinc oxide is used to prevent acne problem rather than treating it. Therefore, it should be used with therapeutic materials such as salicylic acid. Salicylic acid is the only beta-hydroxy acid frequently used in acne treatment due to its ability to open clogged pores and break down fats. While salicylic acid cleanse skin and soothe inflammation, it can cause skin dryness. In the treatment of acne, the use of materials to moisturize the skin can be useful when salicylic acid-containing products are used. Microalgae have been used frequently in the cosmetic industry in recent years for the purpose of moisturizing the skin, removing pale appearance of the skin. Microalgae have Vitamin E, Vitamin B and Vitamin C in their content. Vitamin E helps to moisturize the skin and Vitamin B and Vitamin C help to revitalize the mat and lifeless skin. It also protects the skin against aging due to its proteins, fats, omega, magnesium and zinc. In this study, it is aimed to prevent the spread of acne in human skin by producing nanofiber with electrospinning process. For this purpose, at first zinc oxide nanoparticles (ZnO-NP) were synthesized by microwave irradiation. Synthesized zinc oxide nanoparticles were used in the production of Gelatin/Salicylic Acid/ZnO-NP nanofibers by electrospinning method. ZnO-NP-containing Gelatin/Salicylic Acid/ZnO-NP nanofibers were prepared at various concentrations (%5, 10 and 15) to examine the fiber diameter and surface structure of zinc oxide nanoparticles. Zinc oxide-free Gelatin/Salicylic Acid nano fiber for control and comparison purposes was also produced by electrospinning method. Scanning electron microscope (SEM) was used for comparative examination of surface structures and fiber diameters. The ZnO-NP content of the prepared nanofibers was determined by Energy-dispersive X-ray spectroscopy (EDX). The chemical structures of the prepared nanofibers were analyzed by Fourier Transform Infrared Spectroscopy (FTIR) analysis. In addition, antimicrobial tests of prepared nano fibers against Escherichia coli were performed. Then, the Gelatin/Salicylic acid/Microalgae nanofiber production including Phaeodactylum tricornutum microalgae was performed by electrospinning method. For this purpose, Phaeodactylum tricornutum algae culvitations were prepared and dry algae biomass was obtained from this algae culvitations. The effects of different microalgae concentrations on nanofiber production and structure were investigated. For this purpose, Gelatin/Salicylic acid/Microalgae nanofiber production was performed at different concentrations of microalgae (0.5% and 1%). The surface images and fiber diameters of the produced nano fibers were examined by SEM analysis. Chemical structures of prepared nanofibers were investigated by FTIR analysis. Results were compared with microalgae-free Gelatin / Salicylic Acid control nano fiber. In addition, antimicrobial tests against Escherichia coli were performed for Gelatin/Salicylic acid/Microalgae nano fibers. According to the results of SEM analysis, it was seen that Gelatin/Salicylic Acid/ZnO-NP and Gelatin/Salicylic Acid/Microalgae nano fibers were homogeneous and uniformly distributed. The beads were not found in the fibers. As the percentage of zinc increased in Gelatin/Salicylic acid/ZnO-NP nano fibers, fiber diameters increased. Among nano fibers which are produced, EDX analysis was performed on Gel./SA/5 ZnO nano fiber containing 5% ZnO. The presence of ZnO in produced nano fibers has been proven by EDX analysis. As the percentage of microalgae increased in Gelatin/Salicylic acid/Microalgae nano fibers, fiber diameters decreased. However, fiber diameters of Gelatin/Salicylic Acid control nano fiber was found to be higher than both microalgae concentrations of Gelatin/Salicylic Acid/Microalgae nano fibers. According to the results of antimicrobial tests against Escherichia coli; Gelatin/Salicylic Acid/Microalgae nano fibers have been shown to have antimicrobial properties in both microalgae concentrations. Gelatin/Salicylic Acid/ZnO-NP nano fibers showed no antimicrobial properties at 5% ZnO-NP concentration but showed antimicrobial properties at 10% and 15% ZnO-NP concentrations. The prepared nano fibers melted in the medium and disappeared, but this situation did not affect the test results. When ZnO and SA release tests were performed on the prepared nanofibers, it was seen that the nanofibers melted in the aqueous medium and disappeared. For this reason, it is wanted to be cross-linked these nano fibers. However, it was observed that the nano fibers which were crosslinked in the glutaraldehyde vapor decay and shrink in a very short time. Since nanofiber is intended to be used for multi-use, it is started to be produced Poly caprolactone/Gelatin composite nano fibers without crosslinking. According to the literature researches, it was found that Poly caprolactone (PCL)/Gelatin composite nano fibers showed more advanced properties than the gelatin and PCL nanostructured fibers. When ZnO and SA release tests were performed on the prepared nanofibers, it was seen that the nanofibers melted in the aqueous medium and disappeared. For this reason, it is wanted to be cross-linked these nano fibers. However, it was observed that the nano fibers which were crosslinked in the glutaraldehyde vapor decay and shrink in a very short time. According to the data obtained from the analysis of gelatin nanofibers; it was decided to proceed with the use of Poly Caprolactone (PCL) which can protect the structural integrity of the fiber without the need for any crosslinking agents. According to the literature researches, it was found that Poly caprolactone (PCL)/Gelatin composite nano fibers showed more advanced properties than the gelatin and PCL nanostructured fibers. For the Gel./PCL nanofibers to be produced, the results of the analysis of the pre-prepared Gel./SA/ZnO and Gel./SA/Mikroalg nano fibers were utilized. For the nano fibers to be prepared, 10% ZnO and 1% Microalgae concentration were chosen and firstly Gel./PCL/SA nano fiber was produced by electrospinning for control and comparison purposes. Then, Gel./PCL/SA/10 ZnO nano fiber containing 10% ZnO-NP, Gel./PCL/SA/1 Alg nano fiber containing 1% Phaeodactylum tricornutum microalgae and finally Gel./PCL/SA/10 ZnO / 1 Alg nano fiber containing both 10% ZnO-NP and 1% P Tricornutum microalgae produced by electrospinnig method. Morphological structures and fiber diameters of the nano fibers were analyzed by SEM analysis. The presence of zinc ions in nanofibers containing ZnO-NP was determined by X-ray diffraction (XRD) analysis. Chemical structures of nano fibers were analyzed by FTIR analysis. Antimicrobial tests were performed against Escherichia coli and Staphylococcus aureus bacteria. In addition, zinc ion release and salicylic acid release tests were performed. Finally, the biodegradability test was performed and the water absorption and weight loss values of the produced nano fibers were calculated. According to SEM analysis results, produced nano fibers did not contain beaded structure. It was seen that the surface structures were uniform and homogeneous. SEM analyzes of the produced nano fibers were compared with each other and Gel./PCL/SA control nano fiber. According to the results, it was found that Gel./PCL/SA/10 ZnO nanofiber has the lowest fiber diameter. X-ray diffraction analysis (XRD) has proven the presence of zinc ion in the Gel./PCL/SA/10 ZnO and Gel./PCL/SA/10 ZnO / 1 Algae fibers. According to the results of the antimicrobial test, Gelatin / PCL nanofibers did not show much antimicrobial properties against E. coli and S. aureus. There were no antimicrobial properties against both bacteria for the Gel./PCL/SA control nano fiber. As a result of the antimicrobial test against E. coli, the inhibition diameter of the Gel./PCL/SA/10 ZnO nanofiber containing 10% ZnO was measured and the mean inhibition diameter was found like 1.63. In this case, it can be thought that Jel./PCL/SA/10 ZnO nanofiber has antimicrobial properties against E. coli. As a result of the antimicrobial test performed against S. aureus, it was observed that only Gel./PCL/SA/10 ZnO/1 Alg nano fiber had a small amount of antimicrobial effect with an inhibition diameter of 1.65. According to the results of the releasing tests, it was observed that Gel./PCL nanofibers control the release of zinc oxide and salicylic acid. After the releasing test, the water absorption and weight loss values of the nano fibers which were waited in aqueous media for 7 days were calculated and their biodegradability was investigated. It was found that nano fibers have high water absorption capacity (around 188%) and weight loss values were found around 36% on average. As a result of all productions and analyzes, it was found that Gel./SA and Gel./PCL/SA nano fibers were suitable for use as a face mask for treatment against acne problem. It is more useful to consider the use of Gel./SA nano fibers as single-use because it dissolves in the aqueous medium. In addition it can be said that Gel./PCL/SA nano fibers are suitable for multiple uses.