Electrospun Membranes Research Articles

Hybrid poly(lactide-co-glycolide) membranes incorporated with doxycycline-loaded copper-based metal-organic nanosheets as antibacterial platforms.

The rise of antimicrobial resistance necessitates innovative strategies to combat persistent infections. Metal-Organic Frameworks (MOFs) have attracted significant attention as antibiotic carriers due to their high drug loading capacity and structural adaptability. In particular, 2D MOF nanosheets are emerging as a notable alternative to their traditional 3D relatives due to their remarkable advantages in enhanced surface area, flexibility and exposed active region properties. Herein, we synthesized 2D Copper 1,4-benzendicarboxylate (CuBDC) nanosheets and utilized them as a carrier and controlled release system for Doxycycline (Doxy@CuBDC), for the first time. The Doxy@CuBDC nanosheets were subsequently incorporated into poly (DL-lactide-co-glycolide) (PLGA) electrospun membranes (Doxy@CuBDC/PLGA). The resultant bioactive fibrous membranes exhibited double-barrier controlled release properties, extending the Doxy release up to ∼9 days at pH 7.4 and 5.5. Significant inhibitory effects against Staphylococcus aureus and Escherichia coli were observed. The morphological analyses revealed the deformed bacterial cell structures on Doxy@CuBDC/PLGA membranes that indicates potent bactericidal activity. Furthermore, cytotoxicity assays demonstrated the non-toxic nature of the fabricated membranes, underscoring their potential use for biomedical applications. Overall, the hybrid antibacterial PLGA membranes present a promising strategy for combating microbial infections while maintaining biocompatibility and offer a versatile approach for biomedical material design and surface coatings (e.g., wound dressings, implants).&#xD.

Synergistic Integration of α-Ag2WO4 into PLA/PBAT for the Development of Electrospun Membranes: Advancing Structural Integrity and Antimicrobial Efficacy.

The rising resistance of various pathogens and the demand for materials that prevent infections drive the need to develop broad-spectrum antimicrobial membranes capable of combating a range of microorganisms, thereby enhancing safety in biomedical and industrial applications. Herein, we introduce a simple and efficient technique to engineer membranes composed of polylactic acid (PLA) and polybutylene adipate terephthalate (PBAT) biopolymers and α-Ag2WO4 particles using an electrospinning technique. The corresponding structural, thermal, mechanical, and antimicrobial properties were characterized. X-ray diffraction (XRD) patterns confirmed the integration of crystalline α-Ag2WO4 within the polymer matrix. Scanning electron microscopy (SEM) and Raman confocal microscopy revealed uniformly dispersed α-Ag2WO4 particles in the electrospun fibers, influencing their diameter and surface roughness. Thermal analysis indicated adjustments in the thermal stability and crystallinity of the composites with an increasing α-Ag2WO4 content. Dynamic mechanical analysis (DMA) highlighted variations in storage modulus and glass transition temperatures due to interactions between α-Ag2WO4 and polymer chains, with tensile tests showing an increase in elastic modulus and ultimate tensile strength as the α-Ag2WO4 content increased. Antimicrobial assessments revealed that PLA/PBAT membranes with α-Ag2WO4 showed pronounced antibacterial activity, forming inhibition halos across all samples against Pseudomonas aeruginosa, methicillin-resistant Staphylococcus aureus, and Mycobacterium smegmatis (a surrogate for Mycobacterium tuberculosis). These membranes also exhibited potent antiviral activity against bacteriophage phi 6, a surrogate for SARS-CoV-2, suggesting potential applications in combating infections caused by enveloped viruses. The antimicrobial activities are attributed to the generation of reactive oxygen species (ROS) and the controlled release of Ag+ ions. This work underscores the multifaceted capabilities of α-Ag2WO4-enhanced PLA/PBAT membranes in combating bacterial and viral growth, where both durability and microbial resistance are critical. Taken together, our findings provide a solution for obtaining advanced materials to be applied in a wide range of industrial applications, such as filtration systems, food preservation, antimicrobial coatings, protective textiles, and cleaning products.

Fabrication and adsorption characteristics of cuprammonium cellulose-based membranes for removing anionic and cationic dyes

A cotton linter-based source was used to form conjugate electrospun membranes composed of cuprammonium cellulose, polyethylene oxide, and polyacrylonitrile for the removal of the anionic and cationic dyes from aqueous media. The highest removal efficiencies of 94 %, 89.9 %, 87.4 % were achieved for the anionic dyes Congo red (CR), Metanil yellow (MY), and Methyl orange (MO), respectively, and less so on the cationic dyes Crystal violet (CV), and Rhodamine B (RB) were 55.8 % and 15.1 %, respectively. The pseudo-second-order model effectively described the adsorption kinetics for both types of dyes. The composite membrane exhibited adsorption behaviors following the Dubinin-Radushkevich (D-R) isothermal model. Thermodynamics study suggests that the adsorption process was spontaneous except for the RB dye. The activation energy values of CR, MY, MO, CV, and RB dyes were 27.65, 21.17, 11.50, 10.47, and 71.12 kJ/mol, respectively, confirming the physisorption phenomenon for CR, MY, MO, and CV dyes, while chemisorption occurs for RB dyes. This study investigates the potential of a conjugate electrospun membranes as a reusable adsorbent for dye removal. The effects of solution pH, temperature, and dye concentration on adsorption performance were systematically evaluated. The conjugate electrospun membrane efficiency declined by only 10 % after undergoing five adsorption/desorption cycles.

Molecularly imprinted sensors based on highly stretchable electrospun membranes for cortisol detection

Molecularly imprinted sensors based on highly stretchable electrospun membranes for cortisol detection

Enhancement of antibacterial activity in electrospun fibrous membranes based on quaternized chitosan with caffeic acid and berberine chloride for wound dressing applications.

Electrospun nanofibers made from chitosan are promising materials for surgical wound dressings due to their non-toxicity and biocompatibility. However, the antibacterial activity of chitosan is limited by its poor water solubility under physiological conditions. This study addresses this issue by producing electrospun nanofibers mainly from natural compounds, including chitosan and quaternized chitosan, which enhance both its solubility for electrospinning and the antibacterial activity of the resulting electrospun nanofibers. Additionally, antimicrobial agents like caffeic acid or berberine chloride were incorporated. The glutaraldehyde-treated nanofibers showed improved mechanical properties, with an average tensile strength exceeding 2.7 MPa, comparable to other chitosan-based wound dressings. They also demonstrated enhanced water stability, retaining over 50% of their original weight after one week in phosphate-buffered saline (PBS) at 37 °C. The morphology and performance of these nanofibers were thoroughly examined and discussed. Furthermore, these membranes displayed rapid drug release, indicating potential for inhibiting bacterial growth. Antibacterial assays revealed that S2-CX nanofibers containing caffeic acid were most effective against E. coli and S. aureus, reducing their survival rates to nearly 0%. Similarly, berberine chloride-containing S4-BX nanofibers reduced the survival rates of E. coli and S. aureus to 19.82% and 0%, respectively. These findings suggest that electrospun membranes incorporating chitosan and caffeic acid hold significant potential for use in antibacterial wound dressings and drug delivery applications.

Filtration Performance of Biodegradable Electrospun Nanofibrous Membrane for Sub‐Micron Particles: A Systematic Review

AbstractNanofiber membranes receive considerable interest recently because of their distinctive structural features, facile preparation, as well as high filtering efficiency. Due to ever‐increasing air pollution, membranes made from biodegradable materials can play a crucial part in providing purified air with minimum concerns of environmental issues after the membrane's end of service life. The purpose of this systematic review is to assess the performance of biodegradable electrospun nanofibrous membrane filters toward air sub‐micron particles. To identify relevant studies, a systematic search is carried out in major scientific search engines including PubMed, Scopus, and the Web of Science. Data extraction is used to collect the necessary information on the membranes' structural properties, as well as filtration performance metrics such as efficiency, pressure drop, and quality factor. Among the electrospun membranes derived from biodegradable polymers, the polyvinyl alcohol (PVA)‐based electrospun membranes are more effective in filtration efficiency in capturing sub‐micron particles. The results highlight that these types of membranes are effective in filtration with low energy consumption, making them more apt for air purification. The use of such membranes can supply both high filtering performance and protection of the environment.

Fabrication, Characterization and Release Profile of Aloe Vera Extracts/PVA Composite Electrospun Nanofiber

Aloe vera is a well-known remedy that carries many beneficial health effects such as painkiller, anti-inflammatory, promote skin growth and repair. The combination of bioactive natural product of aloe vera as a drug model and polyvinyl alcohol (PVA) as the base material or carrier in the electrospinning process were studied. Smooth straight and continues electrospun fibers were collected with the Field Effect Scanning Electron Microscope (FESEM) images show no formation of bead (defect signed) in the electrospun membrane when the concentration was set at 10% w/w of PVA nanofibre. The morphological structure of the electrospun membranes shows a smooth and longitudinal fiber when aloe vera is mixed with the PVA polymer with percentage ratio of aloe vera over PVA is less than 25%. The Fourier Transform Infrared Spectroscopy (FTIR) shows no reaction between PVA and aloe vera by not showing peaks other than the initial materials. The Differential Scanning Calorimetry (DSC) proves the presence of aloin indicating the presence of aloe vera in nanofiber. The release profile of the electrospun aloe vera in PVA shows a higher initial burst release at the 50% and 70% concentration levels indicating very little control of the release or none at all. These results show the potential of aloe vera – PVA electrospun nanofibers membrane as a promising material for wound dressing and topical drug delivery.

Effects of Electrospinning Parameters on the Morphology of Electrospun Fibers

Hydrophobic electrospun membranes have a lot of applications in different fields. It is very difficult to increase the hydrophobicity of membranes for a specific application. This study investigates the effects of various electrospinning parameters on the morphology and hydrophobicity of polystyrene (PS) electrospun membranes. Polystyrene fibers were used as a reference for the study. Different parameters such as polymer concentrations, diameter of needles, and applied voltage were tested to study the influence on the hydrophobicity of electrospun fibers. Polystyrene fibers were electrospun at different concentrations from 5 to 20 wt.%, needles with a diameter from 0.5 to 3 mm were used, and voltage was applied between 8.06–16.05 kV. The surface morphology of polystyrene fibers and hydrophobicity were studied with a scanning electronic microscope and contact angle measurements. Based on the results of the study, higher polymer concentrations and voltages produce thinner fibers and more hydrophobic membranes. The results of this paper can be applied to the fabrication of different characteristic membranes for specific applications like water conservation, purification, and other fields.

Electrospun poly(N-vinylpyrrolidone) membranes with Ag nanoparticles for wound dressings: Production and characterization

Wound dressings have long been used to promote the healing of skin injuries. In the work reported here, fibrous membranes were produced by electrospinning poly(N-vinylpyrrolidone) (PVP) solutions containing silver nitrate at varying mass ratios (1:200, 1:100 and 1:50 AgNO3:PVP). PVP solutions without AgNO3 were used as a control. The electrospun membranes were irradiated using 254 nm UV light to simultaneously photo-crosslink PVP and promote the formation of silver nanoparticles (AgNPs). The formation of AgNPs was confirmed by scanning electron microscopy and transmission electron microscopy, as well as by detecting the surface plasmon resonance peak at 420 nm in the UV–Vis spectrum during release studies. The swelling rate of fibrous membranes was lower for those containing AgNPs compared to PVP-only membranes. The Kirby-Bauer diffusion test performed against Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Staphylococcus epidermidis and Candida albicans showed that all AgNPs-containing membranes exhibited an inhibitory effect on all microorganisms tested. The in vitro cytotoxicity assay showed that membranes with lower silver concentration were less cytotoxic. This study presents a simple route to producing a wound dressing with antimicrobial action that has a swelling behavior capable of absorbing exudates, provides controlled release of silver and has low cytotoxicity.

A Polyurethane Electrospun Membrane Loaded with Bismuth Lipophilic Nanoparticles (BisBAL NPs): Proliferation, Bactericidal, and Antitumor Properties, and Effects on MRSA and Human Breast Cancer Cells.

Electrospun membranes (EMs) have a wide range of applications, including use as local delivery systems. In this study, we manufactured a polyurethane Tecoflex™ EM loaded with bismuth-based lipophilic nanoparticles (Tecoflex™ EMs-BisBAL NPs). The physicochemical and mechanical characteristics, along with the antitumor and bactericidal effects, were evaluated using a breast cancer cell line and methicillin-susceptible and resistant Staphylococcus aureus (MRSA). Drug-free Tecoflex™ EMs and Tecoflex™ EMs-BisBAL NPs had similar fiber diameters of 4.65 ± 1.42 µm and 3.95 ± 1.32 µm, respectively. Drug-free Tecoflex™ EMs did not negatively impact a human fibroblast culture, indicating that the vehicle is biocompatible. Tecoflex™ EMs-BisBAL NPs increased 94% more in size than drug-free Tecoflex™ EMs, indicating that the BisBAL NPs enhanced hydration capacity. Tecoflex™ EMs-BisBAL NPs were highly bactericidal against both methicillin-susceptible S. aureus and MRSA clinical isolates, inhibiting their growth by 93.11% and 61.70%, respectively. Additionally, Tecoflex™ EMs-BisBAL NPs decreased the viability of MCF-7 tumor cells by 86% after 24 h exposure and 70.1% within 15 min. Regarding the mechanism of action of Tecoflex™ EMs-BisBAL NPs, it appears to disrupt the tumor cell membrane. In conclusion, Tecoflex™ EMs-BisBAL NPs constitute an innovative low-cost drug delivery system for human breast cancer and postoperative wound infections.

Mechanically Robust and Biodegradable Electrospun Membranes Made from Bioderived Thermoplastic Polyurethane and Polylactic Acid.

Petroleum-based plastic waste plagues the natural environment, but plastics solve many high-performance solutions across industries. For example, porous polymer membranes are used for air filtration, advanced textiles, energy, and biomedical applications. Sustainable and biodegradable Bioplastic membranes can compete with nonrenewable materials in strength, durability, and functionality but biodegrade under select conditions after disposal. Membranes electrospun using a blend of bioderived thermoplastic polyurethane (TPU) and polylactic acid (PLA) perform effectively under tensile and cyclic loading, act adequately as an air filter media, and biodegrade in a home-compost environment, with the aliphatic formulation of TPU showing greater biodegradability compared to the formulation containing aromatic moieties. Blending TPU with PLA dramatically increases the strain at break of the PLA membrane, while the addition of PLA in TPU stiffens the material considerably. Measurements of the pressure drop and filtration efficiency deem this electrospun membrane an effective air filter. This membrane provides a solution to the need for quality air filtration while decreasing the dependence on petroleum feedstocks and addressing the issue of plastic disposal through biodegradation.

Organic-Inorganic Dual-Network Composite Separators for Lithium Metal Batteries.

The suboptimal ionic conductivity of commercial polyolefin separators exacerbates uncontrolled lithium dendrite formation, deteriorating lithium metal battery performance and posing safety hazards. To address this challenge, a novel organic-inorganic composite separator designed is prepared to enhance ion transport and effectively suppress dendrite growth. This separator features a thermally stable, highly porous poly(m-phenylene isophthalamide) (PMIA) electrospun membrane, coated with ultralong hydroxyapatite (HAP) nanowires that promote "ion flow redistribution." The synergistic effects of the nitrogen atoms in PMIA and the hydroxyl groups in HAP hinder anion transport while facilitating efficient Li+ conduction. Meanwhile, the optimized unilateral pore structure ensures uniform ion transport. These results show that the 19µm-thick HAP/PMIA composite separator achieves remarkable ionic conductivity (0.68mS cm-1) and a high lithium-ion transference number (0.51). Lithium symmetric cells using HAP/PMIA separators exhibit a lifespan exceeding 1000h with low polarization, significantly outperforming commercial polypropylene separators. Furthermore, this separator enables LiFePO4||Li cells to achieve an enhanced retention of 97.3% after 200 cycles at 1C and demonstrates impressive rate capability with a discharge capacity of 72.7mAh g-1 at 15C.

PVC/CNT Electrospun Composites: Morphology and Thermal and Impedance Behavior.

Due to their mechanical robustness and chemical resistance, composite electrospun membranes based on polyvinyl chloride (PVC) are suitable for sensor applications. Aiming to improve the electrical characteristics of these membranes, this work investigated the effects of the addition of carbon nanotubes (CNTs) to PVC electrospun membranes, in terms of morphology and thermal and impedance behavior. Transmission electron microscopy images evidenced that most of the nanotubes were encapsulated within the fibers and oriented along them, while field-emission scanning electron micrographs revealed that the membranes consisted of uniform fibers with an average diameter of 339 ± 31 nm, regardless of the addition of the carbon nanotubes. With respect to the neat resin, the addition of nanotubes caused a significant lowering of the glass transition temperature (up to 20 °C) and a marked change in the second degradation step of PVC. Nyquist plots from electrical impedance spectra showed a charge transfer resistance (RCT) of 38 and 40 MΩ for neat PVC and PVC/CNT 3 wt.% membranes, respectively, indicating that, in the dry state, the encapsulation of CNTs in the fibers and the high porosity of the membranes prevented the formation of a percolation network, increasing the electrical resistance. In the wet state, however, there was a greater change in the impedance behavior, decreasing the resistance RCT to 4.5 and 1.1 MΩ, for neat PVC and PVC/CNT 3 wt.% membranes, respectively. The results of this study, showing a significant variation in impedance behavior between dry and wet membranes, are relevant for the development of various types of sensors based on PVC composites.

Electrospun Membranes Modified with Lanmodulin-Derived Peptides for Lanthanide Adsorption

Electrospun Membranes Modified with Lanmodulin-Derived Peptides for Lanthanide Adsorption

Heat-confinement, water-resistance, and moisture-release electrospun membrane based on aerogel filler incorporation

The maintenance of a comparatively stable human body temperature through heating is essential for numerous physiological activities. However, the majority of the existing heating strategies are inefficient and wasteful in terms of energy usage, while also falling short in sufficiently protecting the human body against environmental hazards. Fabrics possessed the abilities to retain heat, repel water, and permit moisture to travel through are in high demand, which are essential for energy conservation and protective purposes. Herein, we introduce a highly efficient approach for producing electrospun membranes that exhibit excellent properties of heat confinement, water repellency, and moisture release properties, achieved by incorporating SiO2 aerogel fillers into interconnected nanofibers. As a result, the obtained aerogel filler incorporation membrane (AFIM) composed of PVDF@SiO2 exhibited a reduced thermal conductivity and reinforced moisture-release capability, leading to a 2 °C increase in temperature differential over its cotton counterpart and a water vapor transmission rate (WVTR) of 26.83 kg•m−2day−1. This work offers insights into the advancement of the thermoregulatory textiles to conserve energy and prevent waterlogging in future challenging conditions.

Preliminary investigation of nanofibrous membranes for sound absorption

Nanofibrous membranes show interesting mechanical properties, low thickness and lightness, besides the possibility of using a great variety of polymers. The electrospinning technique makes possible the production of polymeric random nanofibres to form nonwoven membranes, which are currently used in several application fields, such as filtration, biomedicine, biomechanics, electronics, and composite materials. Their application in the automotive and aerospace engineering field could bring significant benefits to the acoustic comfort design. However, their acoustics properties still need to be further assessed. This study investigates the acoustic absorption of electrospinning-made nanofibrous membranes in Nylon 66 with different fibre diameters and mat thicknesses. Morphological and thermal characterisation of the electrospun membranes have been assessed via Scanning Electron Microscope (SEM) and Differential Scanning Calorimetry (DSC), respectively. The acoustic absorption characteristics of various samples changing fibre diameter, membrane thickness and mounting conditions were tested in the impedance tube. The results showed more relevant acoustic absorption properties in the nanofibrous membrane coupled with a polyester fibre. Further studies will clarify if filament direction and constituent material can be improved for a more durable and resistant membrane application.

Polyhydroxybutyrate/poly(ε‐caprolactone)‐based electrospun membranes loaded with amoxicillin‐potassium clavulanate halloysite nanotubes for biomedical applications

AbstractBiopolymers exhibit distinct properties for biomedical applications. Different biopolymer classes are utilized for various applications, for example antibacterial properties, drug delivery, tissue engineering, tissue scaffolds etc. In the present investigation, a nano‐bioengineering approach was followed to prepare polyhydroxybutyrate and polycaprolactone polymer‐based drug‐loaded halloysite nanotube electrospun membranes for biomedical applications. Functionalized halloysite nanotubes ((3‐aminopropyl)triethoxysilane acid treated halloysite nanotubes) at different weight percentages (1, 3, 5 and 7 wt%) were loaded with a broad‐spectrum antibiotic amoxicillin trihydrate‐potassium clavulanate, incorporated into the electrospun membranes, and characterized by different techniques such as XRD, FTIR, SEM, TEM and TGA. Different physical and mechanical properties were evaluated, such as porosity, water uptake, water vapor transmission rate, wettability and tensile properties. The developed membranes exhibited good in vitro biological properties, for example antibacterial, effective cell migration and less toxicity, as confirmed by disk diffusion, MTT (3‐(4,5‐dimethylthiazolyl‐2)‐2,5‐diphenyltetrazolium bromide) and cell scratch assays. A sustained drug release profile was observed from all the developed membranes. Overall results on the characterization of the developed membranes confirm the suitability of their use for different biomedical applications and as a wound dressing application. © 2024 Society of Chemical Industry.

Enhanced Zinc-air battery performance and local electrochemical evaluation of atomically dispersed Co and Ni in S, N-codoped carbon nanofibers via scanning electrochemical microscopy

This study reports the successful synthesis of a novel electrocatalyst for oxygen reduction reactions (ORR), comprising S,N dual-doped carbon nanofibers with atomically dispersed Co/Ni species (denoted as Co,Ni-SAs/S,N-CNFs), leveraging electrostatic spinning to achieve a unique spatial architecture that maximizes both active site density and mass transport efficiency. Density functional theory (DFT) analysis identified the initial proton-electron transfer to adsorbed O2 as the rate-limiting step, with CoN3S1-NiN3S1 emerging as the pivotal active site structure catalyzing this critical reaction. The fabricated Co,Ni-SAs/S,N-CNFs electrocatalyst exhibited remarkable ORR performance, characterized by a high half-wave potential of 0.84 V and a low Tafel slope of 57.9 mV dec-1. To gain a comprehensive understanding of its catalytic behavior, a tailored temperature-controlled scanning electrochemical microscopy (SECM) was employed, enabling the mapping of reactivity distribution under simulated operating conditions while preserving structural integrity. Liquid zinc-air batteries (ZABs) with this electrocatalyst excelled, reaching 175 mW/cm2 power density and enduring 1240 cycles. The electrospun membrane catalyst enabled both button and flexible ZABs, adaptable to diverse environments. This study advances non-precious metal electrocatalyst design and offers insights for ZAB applications, fostering green energy prospects.

Nanocarrier-Assisted Delivery of Berberine Promotes Diabetic Alveolar Bone Regeneration by Scavenging ROS and Improving Mitochondrial Dysfunction.

Oxidative stress and mitochondrial dysfunction are potential contributors to the compromised tissue regeneration capacity of alveolar bone in diabetic patients. Berberine, an active plant alkaloid, exhibits multiple pharmacological effects including antioxidation, blood glucose- and blood lipid-lowering properties. However, it remains uncertain whether berberine can improve impaired osteogenesis in type 2 diabetes mellitus (T2DM), and its poor solubility and oral bioavailability also constrain its applications in bone regeneration. Thus, our study aimed to probe the effects of berberine on bone marrow stem cells (BMSCs) in a diabetic microenvironment, with a greater emphasis on developing a suitable nano-delivery system for berberine and assessing its capability to repair diabetic alveolar bone defects. Firstly, BMSCs were exposed to berberine within a high glucose and palmitate (HG+PA) environment. Reactive oxygen species levels, mitochondrial membrane potential, ATP generation, cell apoptosis, and osteogenic potential were subsequently assessed. Next, we explored the regulatory mechanism of autophagy flux in the positive effects of berberine. Furthermore, a nanocarrier based on emulsion electrospinning for sustained local delivery of berberine (Ber@SF/PCL) was established. We assessed its capacity to enhance bone healing in the alveolar bone defect of T2DM rats through micro-computed tomography and histology analysis. Berberine treatment could inhibit reactive oxygen species overproduction, mitochondrial dysfunction, apoptosis, and improve osteogenesis differentiation by restoring autophagy flux under HG+PA conditions. Notably, Ber@SF/PCL electrospun nanofibrous membrane with excellent physicochemical properties and good biological safety had the potential to promote alveolar bone remodeling in T2DM rats. Our study shed new lights into the protective role of berberine on BMSCs under T2DM microenvironment. Furthermore, berberine-loaded composite electrospun membrane may serve as a promising approach for regenerating alveolar bone in diabetic patients.

Synthesis of N, N,O and O-carboxymethyl chitosan derivatives of controllable substitution degrees and their utilization as electrospun scaffolds for bone tissue engineering

Most chitosan (CS) carboxymethylation approaches are weighed down by insufficient description protocols regarding the reaction specificity and the degree of substitution (DS). Here, we provide three carboxymethylation protocols of enhanced specificity towards the amine (N-), amine/hydroxy (N,O-) and hydroxy (O-) groups of CS. The DS for all samples was found to be ∼70 %, as confirmed by NMR analysis. To illustrate the modified materials' potential in bone tissue regeneration, each derivative was blended with poly(vinyl alcohol) to prepare scaffolds via electrospinning. Both materials and electrospun membranes were characterized in terms of their physicochemical properties by Fourier transform infrared spectroscopy, thermogravimetric analysis, differential scanning calorimetry and water contact angle measurements. The electrospun membranes' swelling ratio, degradation, tensile strength, as well as morphology were also examined through scanning electron microscopy before and after heat treatment at 120 °C, which was used as a method of physical stabilization, leading to significantly enhanced degradation rate and mechanical strength. The three electrospun scaffold types were loaded with MC3T3-E1 pre-osteoblastic cells and their cell adhesion, viability and growth rate were assessed. Finally, osteogenic differentiation was examined by means of alkaline phosphatase activity measurement, calcium mineralization and formation of extracellular matrix markers, with all materials showing promising prospects.