Electrospinning of polycaprolactone nanofibers using H2O as benign additive in polycaprolactone/glacial acetic acid solution

Considerable efforts have been devoted to the production of polycaprolactone (PCL) nanofibrous structures by electrospinning. However, some toxic solvents have often been used to achieve bead‐free nanofibers. At present, a benign solvent such as glacial acetic acid (GAC) only leads to beaded or microscale fibers. Therefore a study is done to extend the electrospinnability of the PCL/GAC system by the addition of H₂O. The solution properties of conductivity, viscosity, and surface tension were altered by the addition of H₂O, especially increasing the conductivity and viscosity. These properties essential to electrospinning could remain stable for 6 h when the H₂O content was less than or equal to 9 vol %. Then ultrafine PCL fibers with diameters from 188 to 200 nm, 10 times smaller than when dissolved in pure GAC, were electrospun from solutions of PCL with concentrations in the range of 17 to 20 wt % with H₂O content at 9 vol %. Finally, the crystallinity and crystallite size of the resulting fibers were smaller than that of raw PCL pellets. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 45578.     

Electrospinning of gelatin fibers using solutions with low acetic acid concentration: Effect of solvent composition on both diameter of electrospun fibers and cytotoxicity

Gelatin fibers were prepared by electrospinning of gelatin/acetic acid/water ternary mixtures with the aim of studying the feasibility of fabricating gelatin nanofiber mats at room temperature using an alternative benign solvent by significantly reducing the acetic acid concentration. The results showed that gelatin nanofibers can be optimally electrospun with low acetic acid concentration (25%, v/v) combined with gelatin concentrations higher than 300 mg/mL. Both gelatin solutions and electrospun gelatin mats (prepared with different acetic acid aqueous solutions) were analyzed by Fourier transform infrared spectroscopy and differential scanning calorimetry techniques to determine the chemical and structural changes of the polymer. The electrospun gelatin mats fabricated from solutions with low acetic acid content showed some advantages as the maintenance of the decomposition temperature of the pure gelatin (～ 230°C) and the reduction of the acid content on electrospun mats, which allowed to reach a cell viability upper than 90% (analyzed by cell viability test using human dermal fibroblast and embryonic kidney cells). This study has also analyzed the influence of gelatin and acetic acid concentration both on the solution viscosity and the electrospun fiber diameter, obtaining a clear relationship between these parameters. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42115.     

Random and aligned PLLA : PRGF electrospun scaffolds for regenerative medicine

Random and aligned electrospun scaffolds were prepared combining poly(l ‐lactic acid) (PLLA) and activated platelet‐rich plasma (PRGF) at various proportions, with the aim of elucidating the role of nanofibers orientation and growth factors on cell attachment and proliferation. PRGF is released from scaffolds in a sustained way for at least 3 weeks, without an initial burst effect. Mesenchymal stem cells (MSCs) seeded on the random scaffolds present a polygonal and random orientation in any direction of the scaffold. On the other hand, aligned scaffolds are able to promote cell attachment and proliferation in the direction of the nanofibers. The incorporation of PRGF in the scaffolds enhances cell proliferation for at least 2 weeks. Overall, aligned electrospun PLLA : PRGF scaffolds can encapsulate growth factors at relatively large proportions and sustain their release to enhance cell attachment and proliferation as well as eliciting cell alignment. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41372.     

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.     

Core–shell PVA/gelatin nanofibrous scaffolds using co‐solvent,aqueous electrospinning: Toward a green approach

Electrospinning (ES) of gelatin often requires cytotoxic organic solvents or acidic environments, which deteriorate cell recognition sites. In this study, aqueous, non‐toxic, co‐solvent ES was performed to obtain core–shell poly(vinyl alcohol) (PVA)/gelatin nanofiber scaffolds. Effects of the core/shell feed rate ratio (FRR) were investigated on a morphological and mechanical basis. PVA:gelatin ratio of 1:4 was the limiting ratio for specific voltage and electrode distance parameters to obtain uniform fibers. Core–shell bead‐free structures were obtained at 8% PVA and gelatin aqueous solutions. A mean diameter of 280 nm was obtained for 1:1 FRR at 15 kV and 15 cm of electrode distance. Crosslinking resulted in slight improvement in tensile strengths and severe decrease in ductility. Fourier transform infrared spectra revealed retention and improvement of stable secondary structures of gelatin after ES. The scaffolds almost degraded more than 60% in 14 days. Based on the results, present scaffolds hold great promise as suitable candidates for biomedical applications. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46582.     

Composite chitosan/poly(ethylene oxide) electrospun nanofibrous mats as novel wound dressing matrixes for the controlled release of drugs

The aim of this study was to develop novel biomedical electrospun nanofiber mats for controlled drug release, in particular to release a drug directly to an injury site to accelerate wound healing. Here, nanofibers of chitosan (CS), poly(ethylene oxide) (PEO), and a 90 : 10 composite blend, loaded with a fluoroquinolone antibiotic, such as ciprofloxacin hydrochloride (CipHCl) or moxifloxacin hydrochloride (Moxi), were successfully prepared by an electrospinning technique. The morphology of the electrospun nanofibers was investigated by scanning electron microscopy. The functional groups of the electrospun nanofibers before and after crosslinking were characterized by Fourier transform infrared spectroscopy. X‐ray diffraction results indicated an amorphous distribution of the drug inside the nanofiber blend. In vitro drug‐release evaluations showed that the crosslinking could control the rate and period of drug release in wound‐healing applications. The inhibition of bacterial growth for both Escherichia coli and Staphylococcus aureus were achieved on the CipHCl‐ and Moxi‐loaded nanofibers. In addition, both types of CS/PEO and drug‐containing CS/PEO nanofibers showed excellent cytocompatibility in the cytotoxicity assays. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42060.     

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.     

Multifunctional ternary drug‐loaded electrospun scaffolds

Multifunctional electrospun scaffolds were prepared from two polylactide (PLA) grades having slightly different d ‐lactide content (4.2 wt % and 2.0 wt %). Triclosan (TCS), ketoprofen (KTP), and p‐coumaric acid (CUM) were selected as bactericide, anti‐inflammatory, and antioxidant agents, respectively. Single, binary, and ternary drug‐loaded microfibers having a unimodal diameter distribution could be prepared using a common chloroform:acetone:dimethylsulfoxide mixture and similar operational parameters (i.e., voltage, flow rate, and tip–collector distance). FTIR spectra were sensitive to the low amount of drugs loaded and even showed slight differences in PLA conformation. DSC heating scans clearly demonstrated the ability of electrospinning to induce molecular orientation of PLA and also the nucleation effect of incorporated drugs to induce crystallization. Thus, crystallinity of binary drug‐loaded scaffolds was significantly higher than observed for unloaded samples. Release behavior of the three drugs from loaded scaffolds and PLA matrices in PBS:ethanol medium was evaluated. A rapid release was always detected, together with partial drug retention which was higher when the more stereoregular PLA matrix was employed. A strong bactericidal effect was found when scaffolds were loaded with 3 wt/vol % of TCS, but incorporation of a small percentage of KTP (i.e., 1 wt/vol %) had a bacteriostatic effect even in the absence of TCS. The inherent cytotoxicity of TCS could be well neutralized by enhancing cell viability by incorporation of CUM and/or KTP. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 42751.     

Surface modification of electrospun chitosan nanofibrous mats for antibacterial activity

Chitosan (CS) blended with poly(ethylene oxide) (PEO) was electrospun into nanofibrous mats. The spinning solution of 6.7 : 0.3 (% w/v) of CS : PEO was dissolved in a 70 : 30 (v/v) trifluoroacetic acid/dichloromethane solution. The obtained fibers were smooth without beads on their surfaces and average diameter of the fiber was 272 ± 56 nm. N‐(2‐hydroxyl) propyl‐3‐trimethyl ammonium chitosan chloride (HTACC) and N‐benzyl‐N,N‐dimethyl chitosan iodide (QBzCS) were each prepared from the CS/PEO mats. They were identified by Fourier‐transform infrared and X‐ray photoelectron spectroscopy and degree of swelling in water. Both quaternized electrospun chitosan mats exhibited superior antibacterial activity to the unmodified electrospun CS/PEO against Staphylococcus aureus and Escherichia coli at short contact times. After 4 h of contact, the reduction of both bacterial strains by CS/PEO, HTACC, and QBzCS was equal at about 99–100%. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40981.     

Fabrication of PLA/PEG/MWCNT electrospun nanofibrous scaffolds for anticancer drug delivery

In the present study, polylactic acid (PLA)/polyethylene glycol (PEG)/multiwalled carbon nanotube (MWCNT) electrospun nanofibrous scaffolds were prepared via electrospinning process and their applications for the anticancer drug delivery system were investigated. A response surface methodology based on Box–Behnken design (BBD) was used to evaluate the effect of key parameters of electrospinning process including solution concentration, feeding rate, tip–collector distance (TCD) and applied voltage on the morphology of PLA/PEG/MWCNT nanofibrous scaffolds. In optimum conditions (concentration of 8.15%, feeding rate of 0.2 mL/h, voltage of 18.50 kV and TCD of 13.0 cm), the minimum experimental fiber diameter was found to be 225 nm which was in good agreement with the predicted value by the BBD analysis (228 nm). In vitro drug release study of doxorubicin (DOX)‐loaded nanofibrous scaffolds, higher drug content induced an extended release of drug. Also, drug release rate was not dependent on drug/polymer ratio in different electrospun nanofibrous formulations. The equation of M_t = c₀ + kt^0.5was used to describe the kinetic data of DOX release from electrospun nanofibers. The cell viability of DOX‐loaded nanofibrous scaffolds was evaluated using 3‐(4,5‐dimethylthiazol‐2‐yl)‐2,5‐diphenyltetrazolium bromide, a tetrazole assay on lung cancer A549 cell lines. We propose that DOX‐incorporated PLA/PEG/MWCNT nanofibrous scaffold could be used as a superior candidate for antitumor drug delivery. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41286.     

Biocompatible graphene-embedded PCL/PGS-based nanofibrous scaffolds: A potential application for cardiac tissue regeneration

Research in the field of tissue engineering, especially heart tissue engineering, is growing rapidly. Herein, the morphological, chemical, mechanical and biological properties of poly (caprolactone) (PCL)/poly (glycerol sebacate) (PGS) and PCL/PGS/graphene nanofibrous scaffolds are investigated. Initially, PGS pre-polymer is synthesized and characterized by nuclear magnetic resonance and Fourier transform infrared spectroscopies. Then, in order to use the benefits of PGS, this polymer is mixed with PCL. Blending PGS with PCL resulted in the enhancement of ultimate elongation and reduction in the elastic modulus due to the intrinsic properties of PGS. The hydrophobicity of PCL nanofibers is reduced by adding PGS as hydrophilic polymer (105 ± 3° vs. 44 ± 2°). Also, the addition of graphene to the blend nanofibers is balanced the hydrophilicity. Degradation rate of pure PCL nanofibers is very slow but it is increased in the presence of PGS. All nanofibrous scaffolds are biocompatible and non-toxic. The highest cell adhesion (covered area = 0.916 ± 0.032) and biocompatibility (98.79 ± 1%) are related to PCL/PGS loaded with 1% wt of graphene (PCL/PGS/graphene ₁). Thus, this sample can be a good candidate for further examinations of cardiac tissue engineering.     

Characterization and in vitro evaluation of electrospun aligned-fiber membranes of poly(L-co-D,L-lactic acid)

poly(L-co-D,L-lactic acid) (PLDLA) is a bioresorbable and biocompatible copolymer obtained from the combination of L -lactic and D , L -lactic monomers. PLDLA membranes formed by aligned fibers were prepared by AC/DC electrospinning. Solutions of 8 and 10 wt % of PLDLA were used and membranes were collected by a rotating cylindrical collector. The results showed a slight increase in the fiber diameter with the increase in the polymer concentration. Fourier transform infrared spectroscopy results showed no changes in the chemical structure. Dynamic mechanical analysis results showed an increase in the storage modulus and a decrease in glass-transition temperature for the 10 wt % samples, which was corroborated by differential scanning calorimetry. Thermogravimetric analysis showed a slight variation of the peak degradation temperature. Nevertheless, the samples did not present solvent residues. The membranes were tested in vitro using adipose-derived mesenchymal stem cells (ASCs). The ASCs proliferated after 1, 7, and 14 days of culture, maintaining a spindle-like morphology, which evidences their potential for tissue engineering applications. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47657.     

Flurbiprofen axetil loaded coaxial electrospun poly(vinyl pyrrolidone)–nanopoly(lactic‐co‐glycolic acid) core–shell composite nanofibers: Preparation,characterization, and anti‐adhesion activity

Flurbiprofen axetil (FA)‐loaded coaxial electrospun poly(vinyl pyrrolidone) (PVP)–nanopoly(lactic‐co‐glycolic acid) core–shell composite nanofibers were successfully fabricated by a facile coaxial electrospinning, and an electrospun drug‐loaded system was formed for anti‐adhesion applications. The FA, which is a kind of lipid microsphere nonsteroidal anti‐inflammatory drug, was shown to be successfully adsorbed in the PVP, and the formed poly(lactic‐co‐glycolic acid) (PLGA)/PVP/FA composite nanofibers exhibited a uniform and smooth morphology. The cell viability assay and cell morphology observation revealed that the formed PLGA/PVP/FA composite nanofibers were cytocompatible. Importantly, the loaded FA within the PLGA/PVP coaxial nanofibers showed a sustained‐release profile and anti‐adhesion activity to inhibit the growth of the IEC‐6 and NIH3T3 model cells. With the significantly reduced burst‐release profile, good cytocompatibility, and anti‐adhesion activity, the developed PLGA/PVP/FA composite nanofibers were proposed to be a promising material in the fields of tissue engineering and pharmaceutical science. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41982.     

Influence of polycaprolactone/polyglycolide blended electrospun fibers on the morphology and mechanical properties of polycaprolactone

Polycaprolactone (PCL) and polyglycolide (PGA) are two biopolymers that have been used as in situ biomedical devices for various applications. The obstacle of creating a composite that captures the benefit of PCL's long degradation time, while acquiring the strength from PGA is overcoming the lack of surface adhesion between the two biopolymers for stress transfer to occur. This study investigates the use of miscible PCL‐PGA blended fibers, created by electrospinning, to increase the interfacial bonding of fibers to the PCL matrix of the polymer–polymer composite. The use of the blended fibers will thereby create the ability of load transfer from the long‐term PCL matrix to the stronger PCL‐PGA fiber reinforcement. The incorporation of the PCL‐PGA fibers was able to increase the tensile yield strength and Young's modulus over that of the bulk PCL, while decreasing the percent elongation at break. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40224.     

Preparation and surface modification of electrospun aligned poly(butylene carbonate) nanofibers

In this study, aligned poly(butylene carbonate) nanofibers were fabricated by electrospinning with a high‐speed transfer roller as the receiving device. Cold plasma treatment technology was applied to improve its hydrophilicity and activity to expand its application in biological materials. The morphology of the fibers was investigated with scanning electron microscopy. X‐ray diffraction was used to research the impact of the rotation speed on the crystallization and orientation degree of the crystals. The tensile properties of the materials were evaluated by a universal tester. The surface properties of the fibers pretreated by Helium (He) and those grafted with gelatin were evaluated with water contact angle measurement and X‐ray photoelectron spectroscopy. The experimental results indicate that the order degree of fibers, crystallinity, and orientation of the crystalline region, including the mechanical properties, all increased correspondingly with the rotation speed. After plasma pretreatment, the hydrophilicity was improved significantly, and the grafting reaction was realized successfully. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Effects of solvent on structures and properties of electrospun poly(ethylene oxide) nanofibers

Poly(ethylene oxide) (PEO) nanofibers were prepared by electrospinning PEO solution with a mixed solvent of ethanol and deionized water. The results show that the mixed solvent system has noteworthy influences on structures and properties of electrospun PEO nanofibers, including molecular chain orientation, crystallinity degree, surface morphology, fiber diameter, diameter distribution, spinnability, and productivity. With increasing ethanol content in the mixed solvent, wrinkly morphologies appear on the surface of PEO nanofibers due to a high evaporation rate of ethanol during electrospinning process. The dielectric constant, dipole moment, conductivity, density, boiling point, and solubility parameter of the mixed solvent become lower with the ethanol content increasing. Besides, the hydrogen‐bonding interactions between PEO and solvents become weaker. As a result, PEO nanofibers with larger diameters, lower molecular chain orientation, and crystallinity degree are obtained. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 45787.     

Influence of aorta extracellular matrix in electrospun polycaprolactone scaffolds

Cardiovascular disease is the leading cause of mortality worldwide. Therefore, new research strategies for the treatment of cardiovascular disease are required. Previously, extracellular matrices (ECMs) have been used alongside polymers to generate hybrid bioscaffolds. Herein, we propose combining aortic ECMs with a polycaprolactone electrospun scaffold and biomechanically evaluating the scaffolds. We electrospun three scaffolds with varying ECM concentrations and found that increasing the ECM concentration leads to decreased stiffness at low strains, increased elasticity at high strain, reduction in failure strain, and an increase in yield strength. We also noted a decrease in water droplet contact angle with the increasing ECM concentration. Furthermore, we found that all three scaffolds were capable of maintaining human umbilical vein endothelial cell attachment and survival. These findings show the wide spectrum of mechanical properties that can be achieved through the addition of different concentrations of ECM into the fibers. © 2019 The Authors. Journal of Applied Polymer Science published by Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 48181.     

Shape‐memory behaviors of electrospun chitosan/poly(ethylene oxide) composite nanofibrous membranes

With aim of constructing a class of functional environmentally friendly materials, we electrospun chitosan (CS) blends with various contents of poly(ethylene oxide) (PEO) into a series of composite nanofibrous membranes exhibiting shape‐memory behaviors. In the present composite system, CS and PEO served as hard and soft domains, respectively. The CS, presenting no thermal transition, and the PEO, with apparent melting–crystallization, were demonstrated by differential scanning calorimetry testing. Characterizations also revealed that the morphologies of the CS/PEO membranes were controlled by the mass ratios of CS/PEO. The composite fibrous membranes showed great mechanical performances and thermal stabilities as well. Moreover, CS/PEO possessed excellent shape‐memory behaviors. Such fibrous membranes could complete their shape‐recovery processes within 20 s at the temperature of 20°C above the melting transition temperature (T_m). Both the shape fixity and shape‐recovery ratios were higher than 90%, even after five cycles. The CS/PEO fibrous membranes present significant potential applications in the field of biotechnology and tissue engineering, such as in scaffolds and smart tubes. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42532.     

Effect of solution properties on nanofibrous structure of electrospun poly(lactic‐co‐glycolic acid)

Electrospinning of poly(lactic‐co‐glycolic acid) (PLGA) in chloroform or 1,1,1,3,3,3‐hexafluoro‐2‐propanol (HFIP) was investigated, focusing on its solution parameters, to develop nonwoven biodegradable nanofibrous structures for tissue engineering. PLGA nanofibers were obtained by electrospinning of 15 wt % PLGA solution and the resulting average fiber diameters were varied with the range of 270–760 nm, depending on solution property. When small amounts of benzyl triethylammonium chloride (BTEAC) was added to the PLGA/chloroform solution, the average diameter was decreased from 760 to 450 nm and the fibers were densely amounted in a straight shape. In addition, the average fiber diameter (270 nm) of nanofibers electrospun from polar HFIP solvent was much smaller than that (760 nm) of nanofibers electrospun from nonpolar chloroform solvent. Therefore, it could be concluded that conductivity or dielectric constant of the PLGA solution was a major parameter affecting the morphology and diameter of the electrospun PLGA fibers. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 1214–1221, 2006     

Construction of lysozyme exfoliated rectorite‐based electrospun nanofibrous membranes for bacterial inhibition

Lysozyme (LY) exfoliated rectorite (REC) based electrospun nanofibrous membranes with enhanced bacterial inhibition ability and thermostability were fabricated via electrospinning. All the obtained membranes exhibited better fiber shape and three‐dimensional structure, which could be observed by scanning electron microscopy. Energy‐dispersive X‐ray analysis, X‐ray photoelectron spectroscopy, and Fourier transform infrared (FTIR) spectrum denoted the existence of LY and REC in the composite membranes. Besides, the FTIR results suggested that there were interactions between REC and polyvinyl alcohol (PVA)/LY chains. Small angle X‐ray diffraction indicated that REC was exfoliated by PVA and LY chains. In addition, the exfoliation of REC was directly confirmed by transmission electron microscopy. According to Brunauer‐Emmett‐Teller surface area test results, PVA/LY/REC membranes had higher surface area than that of PVA/LY membranes. The performance tests showed that both the thermal stability and antibacterial activity of the composite membranes were enhanced after adding REC. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41496.