Antibacterial polycaprolactone electrospun fiber mats prepared by soluble eggshell membrane protein–assisted adsorption of silver nanoparticles

Antibacterial polycaprolactone (PCL) electrospun fiber mats were prepared by coelectrospinning PCL with soluble eggshell membrane protein (SEP) in 1,1,1,3,3,3‐hexafluoro‐2‐propanol (HFIP), followed by adsorption of silver nanoparticles (Ag NPs) through hydrogen‐bonding interaction between the amide groups of SEP and the carboxylic acid groups capped on the surfaces of Ag NPs. The PCL/SEP fiber mat was characterized by X‐ray photoelectron spectroscopy, indicating the presence of some SEP on the fiber surface. The adsorption of Ag NPs was confirmed by transmission electron microscopy and quantitatively characterized by thermogravimetric analysis. The pH value of the silver sol used for adsorption is very important in view of the amount and dispersion state of Ag NPs adsorbed on the fibers. The Ag NP–decorated PCL/SEP fiber mats prepared at pH 3–5 exhibit strong antibacterial activity against both gram‐negative Escherichia coli and gram‐positive Bacillus subtilis. Antibacterial PCL fiber mats were also obtained similarly with the assistance of collagen (another protein) instead of SEP, showing that protein‐assisted adsorption of Ag NPs is a versatile method to prepare antibacterial electrospun fiber mats. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43850.     

Effect of Thermoplastic Starch and Photocrosslinking on the Properties and Morphology of Electrospun Poly(ethylene-co-vinyl alcohol) Mats

Nonwoven fibrous mats of poly(ethylene-co-vinyl alcohol) (EVOH) and thermoplastic starch (TPS) blends were successfully prepared through the electrospinning technique using a mixed solvent system of isopropyl alcohol and water. The influence of TPS on the morphology and structure of the fibrous mats was investigated using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy. The addition of TPS to EVOH resulted in beaded electrospun fibers. The SEM images revealed decreasing average width of the blend fibers and increasing quantity of beads with an increased TPS content. EVOH/TPS fibers mats irradiated under ultraviolet light using sodium benzoate as a photosensitizer were also prepared. The size and number of beads were diminished in the photocrosslinked EVOH/TPS fiber mats. The as-spun and crosslinked EVOH/TPS fiber mats exhibit a superior fluid uptake ability (with 20 wt% of TPS) and superior barrier properties (with 20 and 40 wt% of TPS) in comparison to those observed in neat electrospun EVOH mats. These properties are of particular interest for use in dressing materials for the medical industry and for use in multilayer plastic fuel tanks for the automotive industry, respectively. POLYM. ENG. SCI., 60:474–480, 2020. © 2019 Society of Plastics Engineers     

Electrospinning polycaprolactone dissolved in glacial acetic acid: Fiber production,nonwoven characterization,and In Vitro evaluation

The electrospinning of polycaprolactone (PCL) dissolved in glacial acetic acid and the characterization of the resultant nonwoven fiber mats is reported in this work. For comparison purposes, PCL fiber mats were also obtained by electrospinning the polymer dissolved in chloroform. Given the processing parameters chosen, results show that 14 and 17 wt % PCL solutions are not viscous enough and yield beaded fibers, 20 and 23 wt % solutions give rise to high quality fibers and 26 wt % solutions yield mostly irregular and fused fibers. The nonwoven mats are highly porous, retain the high tensile strain of PCL, and the fibers are semicrystalline. Cells adhere and proliferate equally well on all mats, irrespective of the solvent used in their production. In conclusion, mats obtained by electrospinning PCL dissolved in acetic acid are also a good option to consider when producing scaffolds for tissue engineering. Moreover, acetic acid is miscible with polar solvents, which may allow easier blending of PCL with hydrophilic polymers and therefore achieve the production of electrospun nanofibers with improved properties. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 41068.     

Fabrication of patterned PDLLA/PCL composite scaffold by electrospinning

Fabricating fibrous electrospun scaffolds with controllable fiber‐arrangement have gained an increasing attention in the field of tissue engineering. In this study, the composite patterned D,L ‐poly(lactic acid)/poly(ε‐caprolactone) (PDLLA/PCL) scaffolds were fabricated via electrospinning for the first time, and the order degree and contractibility of patterned composite scaffolds with different PDLLA/PCL ratios were further investigated. The results showed that the order degree of the pattern and in vitro shrinkage behaviors of PDLLA/PCL electrospun mats could be finely tuned by controlling blending ratios. The PDLLA/PCL electrospun mats with the ratio 50/50 showed the most balanced properties with controllable pattern structure and appropriate dimensional stability, and they might be a suitable candidate for tissue engineering application. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Blending chitosan-g-poly(caprolactone) with poly(caprolactone) by electrospinning to produce functional fiber mats for tissue engineering applications

Use of electrospun fiber mats for tissue engineering applications has become increasingly prominent. One of the most important polymers in research, poly(ε-caprolactone) (PCL), however, lacks biological performance, easy access to modifications and cellular recognition sites. To improve these properties and to enable further modifications, PCL was blended with chitosan grafted with PCL (CS-g-PCL) and subsequently processed via electrospinning. In this way, chitosan was enriched at the fiber's surface presenting cationic amino groups. The fiber mats were analyzed by various techniques such as scanning electron microscopy (SEM), confocal laser scanning microscopy (CLSM), and X-ray photoelectron spectroscopy (XPS). Furthermore, analyzing thermal properties and crystallinity, showed that an increased content of CS-g-PCL in blend composition leads to a higher overall crystallinity in produced fiber mats. Blending CS-g-PCL into PCL significantly increased initial cellular attachment and proliferation as well as cell vitality, while maintaining adequate mechanical properties, fiber diameter, and interstitial volume. As proof of principle for easy access to further modification, fluorescently labeled alginate (Alg-FA) was attached to the fiber's surface and verified by CLSM. Hence, blending CS-g-PCL with PCL can overcome an inherent weakness of PCL and create bioactive implants for tissue engineering applications. © 2019 The Authors. Journal of Applied Polymer Science published by Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48650.     

Electrospinning of poly(hydroxybutyrate‐co‐hydroxyvalerate) fibrous tissue engineering scaffolds in two different electric fields

Poly(hydroxybutyrate‐co‐hydroxyvalerate) (PHBV) was electrospun into ultrafine fibrous nonwoven mats. Different from the conventional electrospinning process, which involves a positively charged conductive needle and a grounded fiber collector (i.e., positive voltage (PV) electrospinning), pseudo‐negative voltage (NV) electrospinning, which adopted a setup such that the needle was grounded and the fiber collector was positively charged, was investigated for making ultrafine PHBV fibers. For pseudo‐NV electrospinning, the effects of various electrospinning parameters on fiber morphology and diameter were assessed systematically. The average diameters of PHBV fibers electrospun via pseudo‐NVs were compared with those of PHBV fibers electrospun via PVs. With either PV electrospinning or pseudo‐NV electrospinning, the average diameters of electrospun fibers ranged between 500 nm and 4 μm, and they could be controlled by varying the electrospinning parameters. The scientific significance and technological implication of fiber formation by PV electrospinning and pseudo‐NV electrospinning in the field of tissue engineering were discussed. POLYM. ENG. SCI., 2011. © 2011 Society of Plastics Engineers     

Fabrication and properties of elastic fibers from electrospinning natural rubber

Electrospinning natural rubber (NR) to get elastic nano-/microfibers has attracted much attention. Suitable solvent such as tetrahydrofuran (THF) was selected by considering solubility, toxicity, and electrospinning results. Dynamic light scattering testing was used to measure the hydrodynamic diameter (D_h) of the solutions with different solvents and the critical concentrations (C*) of NR/THF solution. For NR solutions with the same concentration from different solvents, the larger D_h the solution, the larger the electrospun fiber diameter. Stable electrospinning concentration window ranging from 25 to 50 g/L, which corresponds to 38 > [ŋ]C > 19, was identified. Mechanical properties of both electrospun NR fiber mats and single fibers were estimated from tensile testing. Fibrous mats with excellent elasticity at about 439 to 505% elongation were demonstrated; however, the elongation rate of single fibers was 44%. Electrospun fiber mats with high elasticity of NR materials can be potentially used in soft tissue engineering and strain sensor areas. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 48153.     

Impact of substrate geometry on electrospun fiber deposition and alignment

Aligned, uniform fiber matrixes are highly desirable in numerous engineering and physical science applications. Here, modified electrospinning (ES) deposition substrates (paired and in parallel) are explored to achieve rapid preparation of multiple topographies. Three ES substrates with well‐defined geometries (rectangular, concave, and E‐shaped) were investigated (arranged in parallel) for their impact on fiber size, morphology, orientation, and cell behavior. The results indicate fiber alignment and orientation can be improved and modulated based on the substrate geometry. In addition, altering the interdistance space between various parallel substrates has a clear impact on fiber diameter size and alignment (random, aligned, and perpendicular orientation). Electric field simulations based on substrate geometries show greater probable regions of aligned electric field vectors and distribution, which indicates the most likely deposition attributes of electrospun PCL fibers. Fibrous PCL membranes were biocompatible, and cell growth and guidance were along the fiber path, with evidence of branching at intersecting fibers for multiaxial fibrous topographies. These findings show that the substrate geometry can be optimized to effectively assemble multiaxial layered and well‐aligned fibers in a controlled fashion, which is ideal to support several application developments dependent on fiber topography, integrity, and morphology. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44823.     

Preparation and properties of antibacterial,biocompatible core–shell fibers produced by coaxial electrospinning

Coaxial electrospinning is a method for producing fibrous mats with optional features, such as antibacterial properties, controllable release, and hydrophobicity based on shell materials. Because these features are important in biomedical applications, in this study, biocompatible hydrophobic polymer (polycaprolactone) and hydrophilic polymer [poly(vinyl alcohol)] with silver nanoparticles loaded in the core solution were coaxially electrospun. The effect of silver addition on the conductivity and viscosity of the solutions, chemical structure of the fiber mats, mechanical properties, porosity, hydrophobicity, water vapor transmission rate (WVTR), silver release, and antibacterial properties were investigated. Fibers with silver exhibited less porosity and a lower WVTR and a greater contact angle than the fibers without silver. Furthermore, the core–shell fibers reduced the burst release of silver and successfully prevented the growth of Escherichia coli and Staphylococcus aureus bacteria. Therefore, it seems that these fibers are suitable for providing electrospun mats with long‐term antibacterial properties. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44979.     

Process study,development and degradation behavior of different size scale electrospun poly(caprolactone) and poly(lactic acid) fibers

This study describes the preparation of electrospun poly(caprolactone) (PCL) and poly(lactic acid) (PLA) fibrous scaffolds with and without nano-hydroxyapatite (nHAp) having nanoscale, microscale and combined micro/nano (multiscale) architecture. Processing parameters such as polymer concentration, voltage, flow rate and solvent compositions were varied in wide range to display the effect of each one in determining the diameter and morphology of fibers. The effect of each regulating parameter on fiber morphology and diameter was evaluated and characterized using scanning electron microscope (SEM). Degradability of the selected fibrous scaffolds was verified by phosphate buffered saline immersion and its morphology was analyzed through SEM, after 5 and 12 months. Quantitative measurement in degradation was further evaluated through pH analysis of the medium. Both studies revealed that PLA had faster degradation compared to PCL irrespective of the size scale nature of fibers. Structural stability evaluation of the degraded fibers in comparison with pristine fibers by thermogravimetric analysis further confirmed faster degradability of PLA compared to PCL fibers. The results indicate that PLA showed faster degradation than PCL irrespective of the size-scale nature of fibrous scaffolds, and therefore, could be applied in a variety of biomedical applications including tissue engineering.     

Electrospinning of linear and highly branched segmented poly(urethane urea)s

Electrospun fibrous mats were formed from linear and highly branched poly(urethane urea)s. The highly branched poly(urethane urea)s were synthesized using an A₂+B₃ methodology, where the A₂ species is an oligomeric soft segment. Since the molecular weight of the A₂ oligomer is above the entanglement molecular weight, the highly branched polymers formed electrospun fibers unlike typical hyperbranched polymers that do not entangle. Stress-strain experiments revealed superior elongation for the electrospun fibrous mats. In particular, the highly branched fiber mats did not fail at 1300% elongation, making the electrospun mats promising for potential applications where enhanced tear strength resistance is required.     

Preparation of antibacterial biocompatible polycaprolactone/keratin nanofibrous mats by electrospinning

Keratin-based materials are widely used in biomedical applications due to excellent biocompatibility and biodegradability. In this study, keratin was extracted from waste wool fibers and blended with polycaprolactone (PCL) to produce PCL/keratin nanofibrous mats by electrospinning. The electrospun PCL/keratin nanofibrous mats were chlorinated in diluted sodium hypochlorite solution to endow antibacterial properties. The prepared nanofibrous mats were characterized by scanning electron microscopy, X-ray photoelectron, and Fourier infrared spectroscopy. The effect of the chlorination time on the active chlorine loading of the mats was investigated. The chlorinated PCL/keratin nanofibrous mats with 0.78 ± 0.009 wt% active chlorine displayed potent antibacterial activity against Gram-positive Staphylococcus aureus (ATCC 6538) and Gram-negative Escherichia coli O157:H7 (ATCC 43895) with 6.88 and 6.81 log reductions, respectively. It was found that the mats were compatible with mouse fibroblast cells (L929). The chlorinated PCL/keratin nanofibrous mats might find promising applications in the biomedical field.     

Formation and properties of nylon-6 and nylon-6/montmorillonite composite nanofibers

Nanocomposite fibers of nylon-6 and an organically modified montmorillonite (O-MMT), Cloisite-30B, were prepared by electrospinning. Dispersion and exfoliation of O-MMT in nylon-6 were achieved by melt-extrusion in a twin-screw extruder prior to dissolving in aqueous formic acid for electrospinning. The effects of O-MMT layers on the properties of the nylon-6 solution and electrospun nanocomposite fibers were investigated. Homogeneous, cylindrical nanocomposite fibers with diameters ranging from 70 to 140 nm could be prepared from the 15% composite solution. The O-MMT layers were well exfoliated inside the nanocomposite fibers and were oriented along the fiber direction. Both the degree of nylon-6 crystallinity and the crystallite sizes increased for the nanocomposite fibrous mats, most significantly for those composed of the smallest fibers electrospun from 15% solution. The mechanical properties of the electrospun fibrous mats and single fibers depended not only on the addition of O-MMT layers but also on the sizes of the fibers. Smaller fibers exhibited higher Young's modulus.     

Hybrid biomimetic electrospun fibrous mats derived from poly(ε‐caprolactone) and silk fibroin protein for wound dressing application

To achieve excellent biofunctionality of Bombyx mori silk fibroin (SF), we explored a novel hybridization method to combine the unique properties of SF with poly(ε‐caprolactone) (PCL) electrospun fibers. The hybrid electrospun fibers demonstrate excellent hydrophilicity and biocompatibility that are important to tissue engineering applications. The biomimetic fibrous structure was fabricated by conventional electrospinning of PCL. The individual surfaces of PCL electrospun fibers were coated with silk fibroin protein using a lyophilization technique. The SF coating layers were durable which were further developed by surface modification with fibronectin to improve their biological function. The hybrid electrospun fibers show excellent support for normal human dermal fibroblast (NHDF) cells adhesion and proliferation than neat PCL fibers, while the surface‐modified hybrid electrospun fibers show significantly enhanced proliferation of NHDF cells on their surface. This study indicates the new opportunity of fabrication technique that can construct a biomimetic fibrous structure while the original function as a biomaterial remained existing. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41653.     

Ultrathin electrospun PANI nanofibers for neuronal tissue engineering

N‐(4‐aminophenyl)aniline oxidative polymerization is optimized to produce polyaniline (PANI) free from carcinogenic and/or polluting coproducts. The resulting polymer is electrospun using polymethyl methacrylate (PMMA) as the supporting polymer, with different weight ratios (1:0, 4:1, 3:1, 2:1, 1:1, and 0.5:1 w/w PANI/PMMA). By rinsing with a selective solvent, PMMA is removed while maintaining the fibrous morphology. Ultrathin (65 ± 14 nm) and defect‐free PANI nanofiber mats are obtained for the blend containing a high relative content of PANI (2:1 w/w, namely F_2:1). Two different solvents are tested to remove PMMA, namely acetone and isopropanol, the former giving better results, as highlighted by infrared spectroscopy (FTIR). X‐ray diffraction (XRD) demonstrates that the electrospun PANI is amorphous. The thin fiber mats are robust and sterilization both by autoclave and UV irradiation can be carried out. UV irradiation is preferred since no modification of the fibrous morphology is detectable. In vitro biocompatibility of the electrospun F_2:1 fibers has been evaluated with SH‐SY5Y neuronal‐like cells. Indirect cytocompatibility tests show that no cytotoxic leachable is released by the electrospun mats at both short and longer times, while direct cytocompatibility investigations indicate that only F_2:1 fibers washed in isopropanol do not reduce cell proliferation rate with respect to controls on tissue culture plates. Globally, these results suggest that the proposed electrospun nanostructures are promising materials for neuronal tissue engineering. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43885.     

Fabrication and characterization of electrospun polybutadiene fibers crosslinked by UV irradiation

Crosslinked electrospun polybutadiene (BR) fibers were made using electrospinning and UV curing methods. The crosslinked BR fibers were obtained by irradiating UV light on the electrospun BR fibers containing a photoinitiator and a crosslinker. Although uncrosslinked electrospun BR fibers did not retain the fiber morphology at room temperature due to a cold flow resulting from the very low glass transition temperature (T_g) of BR (below ?80°C), the crosslinked electrospun BR fibers retained the fiber morphology. The crosslink density increased with increase of the content of crosslinking agent. The crosslinked BR fibers had higher T_g than the raw BR. Tensile strength, modulus, and elongation at break of the electrospun BR fiber mats increased with increase of the crosslinker content. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 2233–2337, 2006     

Point‐bonded electrospun polystyrene fibrous mats fabricated via the addition of poly(butylacrylate) adhesive

Because of poor mechanical strength, applications of electrospun polystyrene (PS) fibrous mats are quite limited. The introduction of various concentrations of poly (butylacrylate) adhesives (PBAs) into PS solutions led to the fabrication of point‐bonded electrospun PS fibrous mats with good mechanical strength. The morphologies of PS/PBA fibers with varying PBA content (0?50 wt%) were investigated using scanning electron microscopy (SEM), and the results were compared with pure PS and PBA fibers fabricated with various solvents. SEM images indicated that point‐bonded PS/PBA fibers were uniformly distributed with an average diameter of 1–2 μm. On increasing concentration of PBA up to 20 wt%, porous PS/PBA fibrous mats were obtained. However, solid films were formed at very high concentrations of PBA. The Young's modulus and tensile strength of PS/PBA fibrous mats increased up to 52.4 and 2.7 MPa, respectively. The resultant enhancement of the mechanical properties of PS fibrous mats on addition of PBA increases the number of potential applications of these materials. POLYM. ENG. SCI., 2011. © 2011 Society of Plastics Engineers     

Improvement of carbon nanotube dispersion in electrospun polyacrylonitrile fiber through plasma surface modification

In this study, surfaces of multiwalled carbon nanotubes (CNTs) were functionalized with poly(hexafluorobutyl acrylate) (PHFBA) thin film using a rotating-bed plasma-enhanced chemical vapor deposition (PECVD) method without imparting any defects on their surfaces. Polyacrylonitrile (PAN) electrospun polymer fiber mats and composite fiber mats with CNTs and functionalized CNTs (f-CNTs) were prepared. The wettability and chemical and morphological properties of the synthesized fiber mats were investigated, and the dispersion of CNTs and f-CNTs in the polymer matrix was compared according to the contact angle results of electrospun polymer mats. According to the chemical and morphological characterization results, PHFBA-coated CNTs were dispersed more uniformly in the polymer matrix than the uncoated CNTs. The f-CNTs/PAN composite fiber mat exhibits a lower surface energy than the pristine CNTs/PAN fiber mat. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47768.     

Functionally modified,melt‐electrospun thermoplastic polyurethane mats for wound‐dressing applications

The electrospinning of a polymer melt is an interesting process for medical applications because it eliminates the cytotoxic effects of solvents in the electrospinning solution. Wound dressings made from thermoplastic polyurethane (TPU), particularly as a porous structured electrospun membrane, are currently the focus of scientific and commercial interest. In this study, we developed a functionalized fibrillar structure as a novel antibacterial wound‐dressing material with the melt‐electrospinning of TPU. The surface of the fibers was modified with poly(ethylene glycol) (PEG) and silver nanoparticles (nAg's) to improve their wettability and antimicrobial properties. TPU was processed into a porous, fibrous network of beadless fibers in the micrometer range (4.89 ± 0.94 μm). The X‐ray photoelectron spectroscopy results and scanning electron microscopy images confirmed the successful incorporation of nAg's onto the surface of the fiber structure. An antibacterial test indicated that the PEG‐modified nAg‐loaded TPU melt‐electrospun structure had excellent antibacterial effects against both a Gram‐positive Staphylococcus aureus strain and Gram‐negative Escherichia coli compared to unmodified and PEG‐modified TPU fiber mats. Moreover, modification with nAg's and PEG increased the water‐absorption ability in comparison to unmodified TPU. The cell viability and proliferation on the unmodified and modified TPU fiber mats were investigated with a mouse fibroblast cell line (L929). The results demonstrate that the PEG‐modified nAg‐loaded TPU mats had no cytotoxic effect on the fibroblast cells. Therefore, the melt‐electrospun TPU fiber mats modified with PEG and nAg have the potential to be used as antibacterial, humidity‐managing wound dressings. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40132.     

Electrospun 1,6-diisocyanatohexane-extended poly(1,4-butylene succinate) fiber mats and their potential for use as bone scaffolds

Ultrafine 1,6-diisocyanatohexane-extended poly(1,4-butylene succinate) (PBSu-DCH) fibers were best fabricated by electrospinning from 22% w/v PBSu-DCH solution in 90:10 v/v dichloromethane/trifluoroacetic acid under the electric field of 17 kV/20 cm. The diameters of these fibers were 172 ± 3 nm. Due to their fibrous nature, the obtained PBSu-DCH fiber mats exhibited high values of advancing/receding water contact angles (i.e., 114°/79°) and porosity (69%). Indirect cytotoxicity evaluation of the PBSu-DCH fiber mats based on the viabilities of human osteosarcoma cells (SaOS-2) and mouse fibroblasts (L929) revealed that the fibrous materials did not release any substance in the level that was harmful to the cells. The potential for use of the PBSu-DCH fiber mats as substrates for bone cell culture was further evaluated in vitro with SaOS-2 in terms of the ability to support the attachment and to promote the proliferation and the differentiation of the seeded/cultured cells. Comparative studies were made against corresponding solvent-cast PBSu-DCH films. The results indicated that the bone cells grown on the surface of the fiber mats could attach, proliferate and express alkaline phosphatase (ALP), an early osteogenic proliferation marker, better than they did on the surface of the films. The evidence obtained in this work implies the potential for use of the electrospun PBSu-DCH fiber mats as bone scaffolds.