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The effect of low-temperature arc discharge plasma treatment in a nitrogen atmosphere on the modification of the physicochemical properties of PLA-based scaffolds was studied. In addition, the cellular-mediated immune response when macrophages of three donors interact with the modified surfaces of PLA-based scaffolds was investigated. PLA surface carbonization, accompanied by a carbon atomic concentration increase, was revealed to occur because of plasma treatment. Nitrogen plasma significantly influenced the PLA wettability characteristics, namely, the hydrophilicity and lipophilicity were improved, as well as the surface energy being raised. The viability of cells in the presence of the plasma-modified PLA scaffolds was evaluated to be higher than that of the initial cells.

We studied restoration of microvessels in the oral mucosa wound defects under a polymer piezoelectric membrane (group 2) and without it (group 1). The control group included animals with intact mucosa. On day 3, the expression of the vascular endothelial growth factor (VEGF) increased in all experimental groups, while the expression of CD34 increased only in group 2, which attested to intensive neoangiogenesis. On day 7, we observed a decrease in VEGF expression and an increase in CD34 expression that was more pronounced in group 2, which reflected the beginning of blood vessels maturation. More rapid formation and maturation of blood vessels in group 2 was confirmed by electron microscopy: on day 7, endothelial cells with mature organelles and signs of active transcapillary exchange were seen. On day 12, the immature blood vessels still predominated in group 1, while in group 2, the expression of angiogenesis markers decreased though remained above the control, which created prerequisites for the complete restoration of wound area vascularization in group 2. In group 1, the expression of VEGF and CD34 was significantly below the control, which attested to the development of poorly vascularized scar tissue., (© 2023. Springer Science+Business Media, LLC, part of Springer Nature.)

In this work, the micro-arc oxidation method is used to fabricate surface-modified complex-structured titanium implant coatings to improve biocompatibility. Depending on the utilized electrolyte solution and micro-arc oxidation process parameters, three different types of coatings (one of them-oxide, another two-calcium phosphates) were obtained, differing in their coating thickness, crystallite phase composition and, thus, with a significantly different biocompatibility. An analytical approach based on X-ray computed tomography utilizing software-aided coating recognition is employed in this work to reveal their structural uniformity. Electrochemical studies prove that the coatings exhibit varying levels of corrosion protection. In vitro and in vivo experiments of the three different micro-arc oxidation coatings prove high biocompatibility towards adult stem cells (investigation of cell adhesion, proliferation and osteogenic differentiation), as well as in vivo biocompatibility (including histological analysis). These results demonstrate superior biological properties compared to unmodified titanium surfaces. The ratio of calcium and phosphorus in coatings, as well as their phase composition, have a great influence on the biological response of the coatings.

Biodegradable polymeric fibrous non-woven materials are widely used type of scaffolds for tissue engineering. Their morphology and properties could be controlled by composition and fabrication technology. This work is aimed at development of fibrous scaffolds from a multicomponent polymeric system containing biodegradable synthetic (polylactide, polycaprolactone) and natural (gelatin, chitosan) components using different methods of non-woven mats fabrication: electrospinning and electro-assisted solution blow spinning. The effect of the fabrication technique of the fibrous materials onto their morphology and properties, including the ability to support adhesion and growth of cells, was evaluated. The mats fabricated using electrospinning technology consist of randomly oriented monofilament fibers, while application of solution blow spinning gave a rise to chaotically arranged multifilament fibers. Cytocompatibility of all fabricated fibrous mats was confirmed using in vitro analysis of metabolic activity, proliferative capacity and morphology of NIH 3T3 cell line. Live/Dead assay revealed the formation of the highest number of cell-cell contacts in the case of multifilament sample formed by electro-assisted solution blow spinning technology.

In this study, polymer scaffolds were fabricated from biodegradable poly(lactide-co-glycolide) (PLGA) and from non-biodegradable vinylidene fluoride-tetrafluoroethylene (VDF-TeFE) by electrospinning. These polymer scaffolds were subsequently surface-modified by sputtering titanium targets in an argon atmosphere. Direct current pulsed magnetron sputtering was applied to prevent a significant influence of discharge plasma on the morphology and mechanical properties of the nonwoven polymer scaffolds. The scaffolds with initially hydrophobic properties show higher hydrophilicity and absorbing properties after surface modification with titanium. The surface modification by titanium significantly increases the cell adhesion of both the biodegradable and the non-biodegradable scaffolds. Immunocytochemistry investigations of human gingival fibroblast cells on the surface-modified scaffolds indicate that a PLGA scaffold exhibits higher cell adhesion than a VDF-TeFE scaffold.

We studied the features of hydrolytic degradation of polylactic acid (PLLA) implants depending on their structural filling with hydroxyapatite (HA). The resistance to in vitro hydrolysis was tested for the following samples: PLLA without HA (control; group 1), PLLA/HA 25 wt% (group 2), and PLLA/HA 50 wt% (group 3). Samples were incubated at 37°C. In the hydrolysate, lactate, calcium ions, and inorganic phosphate were determined. Additionally, the time of appearance of visual deformation and sample disintegration was recorded. PLLA degradation was higher in samples saturated with HA. The highest resistance to deformation was noted for samples without HA. Samples with a PLLA/HA 50 wt% demonstrated the maximum degradation of PLLA in combination with lower resistance to deformation and the highest bioavailability of calcium and phosphate. Group 2 samples are most promising for clinical use., (© 2022. Springer Science+Business Media, LLC, part of Springer Nature.)

In the present study, wound healing ferroelectric membranes doped with zinc oxide nanoparticles were fabricated from vinylidene fluoride-tetrafluoroethylene copolymer and polyvinylpyrrolidone using the electrospinning technique. Five different ratios of vinylidene fluoride-tetrafluoroethylene to polyvinylpyrrolidone were used to control the properties of the membranes at a constant zinc oxide nanoparticle content. It was found that an increase of polyvinylpyrrolidone content leads to a decrease of the spinning solution conductivity and viscosity, causing a decrease of the average fiber diameter and reducing their strength and elongation. By means of X-ray diffraction and infrared spectroscopy, it was revealed that increased polyvinylpyrrolidone content leads to difficulty in crystallization of the vinylidene fluoride-tetrafluoroethylene copolymer in the ferroelectric β-phase in membranes. Changing the ratio of vinylidene fluoride-tetrafluoroethylene copolymer and polyvinylpyrrolidone with a constant content of zinc oxide nanoparticles is an effective approach to control the antibacterial properties of membranes towards Staphylococcus aureus . After carrying out in vivo experiments, we found that ferroelectric hybrid membranes, containing from five to ten mass percent of PVP, have the greatest wound-healing effect for the healing of purulent wounds.

Composite poly-L-lactide acid-based scaffolds with hydroxyapatite (HAp) content up to 75 wt.% were fabricated via solution blow spinning. The influence of HAp concentration on structure, wettability, mechanical properties and chemical and phase composition of the produced materials was examined. It was found that with an increase of HAp content the average fiber diameter was increased, the uniaxial strength and relative elongation were reduced, while the phase composition and surface wettability did not change. The performance of the scaffolds during implantation in the parietal bone of a rat skull for a period from 15 to 90 days was studied. The materials have shown high ability to integrate with both soft and hard tissues. It was found that scaffolds with 25 wt.% HAp content significantly enhance osteogenesis during scarification (damage) of the periosteum. Overall, the fabricated scaffolds proved to be highly efficient for replacing bone defects in long tubular bones., (© 2021 IOP Publishing Ltd.)

The aim of the investigation was to study the influence of pore size and the presence of a biologically active calcium phosphate coating in porous 3D printed titanium implants on the process of integration with the bone tissue., Materials and Methods: Samples of cylindrical implants with three different pore diameters (100, 200, and 400 μm) were fabricated from titanium powder on the Arcam 3D printer (Sweden) using electron beam melting technology. A calcium phosphate coating with a thickness of 20±4 μm was applied to some of the products by microarc oxidation. Cytotoxicity of the implants was determined in vitro on human dermal fibroblast cultures. The samples were implanted in the femoral bones of 36 rabbits in vivo . The animals were divided into 6 groups according to the bone implant samples. The prepared samples and peri-implant tissues were studied on days 90 and 180 after implantation using scanning electron microscopy and histological methods., Results: All samples under study were found to be non-toxic and well biocompatible with the bone tissue. There were revealed no differences between coated and non-coated implants of 100 and 200 μm pore diameters in terms of their histological structure, intensity of vascularization in the early stages, and bone formation in the later stages. Samples with pore diameters of 100 and 200 μm were easily removed from the bone tissue, the depth of bone growth into the pores of the implant was lower than in the samples with pore diameter of 400 μm (p<0.001). There were differences between coated and non-coated samples of 400 μm pore diameter, which was expressed in a more intensive osseointegration of samples with calcium phosphate coating (p<0.05)., Conclusion: The optimal surface characteristics of the material for repairing bone defects are a pore diameter of 400 μm and the presence of a calcium phosphate coating., Competing Interests: Conflict of interest. OSTEOMED-M LLC (Moscow) develops and manufactures implants and instruments for traumatology, orthopedics, endoprosthetics, and spinal surgery. OSTEOMED-M LLC had no influence on the results of the study.

Wound healing is a complex process and an ongoing challenge for modern medicine. Herein, we present the results of study of structure and properties of ferroelectric composite polymer membranes for wound healing. Membranes were fabricated by electrospinning from a solution of vinylidene fluoride/tetrafluoroethylene copolymer (VDF-TeFE) and polyvinylpyrrolidone (PVP) in dimethylformamide (DMF). The effects of the PVP content on the viscosity and conductivity of the spinning solution, DMF concentration, chemical composition, crystal structure, and conformation of VDF-TeFE macromolecules in the fabricated materials were studied. It was found that as PVP amount increased, the viscosity and conductivity of the spinning solutions decreased, resulting in thinner fibers. Using FTIR and XRD methods, it was shown that if the PVP content was lower than 50 wt %, the VDF-TeFE copolymer adopted a flat zigzag conformation (TTT conformation) and crystalline phases with ferroelectric properties were formed. Gas chromatography results indicated that an increase in the PVP concentration led to a higher residual amount of DMF in the material, causing cytotoxic effects on 3T3L1 fibroblasts. In vivo studies demonstrated that compared to classical gauze dressings impregnated with a solution of an antibacterial agent, ferroelectric composite membranes with 15 wt % PVP provided better conditions for the healing of purulent wounds.

These days, composite materials based on polymers and inorganic nanoparticles (NPs) are widely used in optoelectronics and biomedicine. In this work, composite membranes of polylactic acid and ZnO NPs containing 5-40 wt.% of the latter NPs were produced by means of electrospinning. For the first time, polymer material loaded with up to 40 wt.% of ZnO NPs (produced via laser ablation in air and having non-modified surface) was used to prepare fiber-based composite membranes. The morphology, phase composition, mechanical, spectral and antibacterial properties of the membranes were tested by a set of analytical techniques including SEM, XRD, FTIR, UV-vis, and photoluminescence spectroscopy. Antibacterial activity of the materials was evaluated following standard procedures (ISO 20743:2013) and using S. aureus and E. coli bacteria. It is shown that incorporation of 5-10 wt.% of NPs led to improved mechanical properties of the composite membranes, while further increase of ZnO content up to 20 wt.% and above resulted in their noticeable deterioration. At the same time, the antibacterial properties of ZnO-rich membranes were more pronounced, which is explained by a larger number of surface-exposed ZnO NPs, in addition to those embedded into the bulk of fiber material.

Direct current (DC) reactive magnetron sputtering is as an efficient method for enhancing the biocompatibility of poly(ε-caprolactone) (PCL) scaffolds. However, the PCL chemical bonding state, the composition of the deposited coating, and their interaction with immune cells remain unknown. Herein, we demonstrated that the DC reactive magnetron sputtering of the titanium target in a nitrogen atmosphere leads to the formation of nitrogen-containing moieties and the titanium dioxide coating on the scaffold surface. We have provided the possible mechanism of PCL fragmentation and coating formation supported by XPS results and DFT calculations. Our preliminary biological studies suggest that DC reactive magnetron sputtering of the titanium target could be an effective tool to control macrophage functional responses toward PCL scaffolds as it allows to inhibit respiratory burst while retaining cell viability and scavenging activity.

The modulation of phagocyte responses is essential for successful performance of biomaterials in order to prevent negative outcomes associated with inflammation. Herein, we developed electrospun poly(ε-caprolactone) (PCL) scaffolds doped with the novel potent c-Jun N-terminal kinase (JNK) inhibitors 11 H -indeno[1,2- b ]quinoxalin-11-one oxime ( IQ-1 ) and 11 H -indeno[1,2- b ]quinoxalin-11-one O -( O -ethylcarboxymethyl) oxime( IQ-1E ) as a promising approach for modulating phagocyte activation. Optimized electrospinning parameters allowed us to produce microfiber composite materials with suitable mechanical properties. We found that embedded compounds were bound to the polymer matrix via hydrophobic interactions and released in two steps, with release mostly controlled by Fickian diffusion. The fabricated scaffolds doped with active compounds IQ-1 and IQ-1E effectively inhibited phagocyte inflammatory responses. For example, they suppressed human neutrophil activation by the biomaterials, as indicated by decreased neutrophil reactive oxygen species (ROS) production and Ca 2+ mobilization. In addition, they inhibited lipopolysaccharide (LPS)-induced NF-κB/AP-1 reporter activity in THP-1Blue cells and interleukin (IL)-6 production in MonoMac-6 cells without affecting cell viability. These effects were attributed to the released compounds rather than cell-surface interactions. Therefore, our study demonstrates that doping tissue engineering scaffolds with novel JNK inhibitors represents a powerful tool for preventing adverse immune responses to biomaterials as well as serves as a platform for drug delivery.

In the present study, we report a simple and efficient method of gelatin immobilization on the surface of PLA electrospun fibers using pre-treatment with a mixture of toluene and ethanol allowing to form swelled surface layer followed by gelatin adsorption from its solution in PBS. Our results demonstrate that gelatin immobilization leads to a decrease in the water contact angle from 120° to 0°, enhances scaffold strength up to 50%, and doubles the number of adhered cells and their average area. We observed that the maximum amount of gelatin (0.07 ± 0.01 mg per cm 3 of the scaffold) was immobilized during the first five minutes of exposure to the gelatin solution. Modified scaffolds demonstrated increased strength., (Copyright © 2019 Elsevier B.V. All rights reserved.)

This study aims to investigate the comparative study of calcium phosphate coatings for flexible intramedullary nails (FINs) used to lengthen long tubular bones. The presence of a calcium phosphate coating deposited by micro-arc oxidation (MAO) or a composite coating based on a co-polymer of vinylidene fluoride with tetrafluoroethylene (VDF-TeFE) and hydroxyapatite (HA) on the surface of the FIN significantly enhanced the regeneration of bone in the area of osteotomy during limb lengthening by combined osteosynthesis. The investigation of the physico-chemical properties of the FIN coated with calcium phosphate via MAO demonstrated that the improved bone tissue formation resulted from favourable conditions for adhesion, proliferation and differentiation of multipotent stem cells into osteoblasts on the coating surface. The composite coatings only stimulated the formation of bone tissue in vivo, primarily because of the piezoelectric properties of the VDF-TeFE co-polymer.

Early treatment of bone fractures was performed using implants, which are often used in the form of plates of various types, which are fixed on the bone surface (extracellular fixation) and nails that are located in the medullary canal (intracerebral fixation). The goal of this study was to investigate the features of osseointegration of implants for internal fixation (intramedullary or extramedullary) with various bioactive coating techniques. During experimental study on 20 mongrel dogs, the implant model in the form of 1.0-mm plate made of titanium alloy (Ti6Al 4V) was placed in the medullary canal (first series) or under the periosteum (second series): the plates had bioactive coating (hydroxyapatite) produced using the technology of magnetron sputtering (six animals), plasma electrolytic oxidation or microarc oxidation technology (PEO; eight animals), and composite technology (six dogs). Anatomic and histological studies have shown that the process of active osseointegration of porous implants with bioactive coating begins after 7 days: at first, granulation tissue - and then fibrous connective tissue - is formed; after 14 days, the osteogenic substrate can be found, and after 28 days, the entire implant area is covered by the lamellar bone tissue, which creates single implant-bone block. The most active formation of bone tissue is observed around implants with bioactive coating produced using the last two technologies. Low traumatic placement of porous implants with bioactive coating in the medullary canal or subperiosteally provides the stimulation of reparative osteogenesis and rapid (especially with PEO technique) osseointegration of the implant., (© 2018 John Wiley & Sons, Ltd.)

In this study, thin calcium phosphate (Ca-P) coatings were deposited on zirconia substrates by radiofrequency (RF) magnetron sputtering using different calcium phosphate targets (calcium phosphate tribasic (CPT), hydroxyapatite (HA), calcium phosphate monobasic, calcium phosphate dibasic dehydrate (DCPD) and calcium pyrophosphate (CPP) powders). The sputtering of calcium phosphate monobasic and DCPD powders was carried out without an inert gas in the self-sustaining plasma mode. The physico-chemical, mechanical and biological properties of the coatings were investigated. Cell adhesion on the coatings was examined using mesenchymal stem cells (MSCs). The CPT coating exhibited the best cell adherence among all the samples, including the uncoated zirconia substrate. The cells were spread uniformly over the surfaces of all samples., Competing Interests: The authors declare no conflict of interest.

In this study, we modified the surface of bioresorbable electrospun poly-(l-lactic) acid (PLLA) scaffolds by reactive magnetron sputtering of a titanium target under a nitrogen atmosphere. We examined the influence of the plasma treatment time on the structure and properties of electrospun PLLA scaffolds using SEM, XRF, FTIR, XRD, optical goniometry, and mechanical testing. It was observed that the coating formed did not change physicomechanical properties of electrospun PLLA scaffolds and simultaneously, increased their hydrophilicity. No adverse tissue reaction up to 3 months after subcutaneous implantation of the modified scaffolds was detected in in-vivo rat model. The rate of scaffold replacement by the recipient tissue in-vivo was observed to depend on the plasma treatment time., (Copyright © 2017 Elsevier B.V. All rights reserved.)

We studied the possibility of seeding bone marrow-derived stromal cells onto polylactic acid-based scaffolds fabricated by electrospinning and solution blow spinning technologies. The cells were applied to the scaffolds by dynamic seeding and scaffolds were then cultured in Petri dishes in culture medium for 3 days. Cell migration to the Petri dish surface was noted only for scaffolds fabricated by electrospinning technology, but DAPI staining confirmed the presence of cells in both scaffolds. The mean number of cells in scaffolds fabricated by electrospinning and solution blow spinning was 56±9 and 81±6, respectively. The scaffold fabricated by solution blow spinning was more effectively (p<0.05) colonized by cells due to its more optimal spatial structure.

This work presents composite coatings based on a copolymer of vinylidene fluoride with tetrafluoroethylene (VDF-TeFE) and hydroxyapatite (HA) for flexible intramedullary nails (FIN). The effect of the proportion of VDF-TeFE (100-25% wt.) on physicochemical and biological properties of the composite coatings was investigated. It was shown that a decrease of VDF-TeFE in the coating hinders its crystallization in β and γ forms which have piezoelectric properties. The decrease also reduces an adhesive strength to 9.9±2.4MPa and a relative elongation to 5.9±1.2%, but results in increased osteogenesis. It was demonstrated that the composite coatings with 35% VDF-TeFE has the required combination of physicochemical properties and osteogenic activity. Comparative studies of composite coatings (35% VDF-TeFE) and calcium phosphate coatings produced using micro-arc oxidation, demonstrated comparable results for strength of bonding of these FINs with trabecular bones (~530MPa). It was hypothesized that the high osteoinductive properties of the composite coatings are due to their piezoelectric properties., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Surface modification of bioresorbable polymer material (polycaprolactone, PCL) with abnormal glow discharge, initiated during radio-frequency magnetron sputtering of a hydroxyapatite target was investigated. Plasma treatment resulted in an increase of surface roughness of PCL, crystallite size, the surface free energy and hydrophilicity. Increased treatment time (30, 60, 150 seconds) provoked the polymer surface saturation with the sputtering target ions (calcium, phosphorus). The assessment of plasma exposure of PCL surface on bone marrow multipotent mesenchymal stromal cells behavior (BM MSCs) has been performed. Modification of the polymer surface with the abnormal glow discharge stimulated adhesion and subsequent proliferation of BM MSCs; thus, maximum values were achieved with the surface treatment for 60 s. This type of plasma modification did not affect cell viability (apoptosis, necrosis). Thus, the surface modification with abnormal glow discharge, initiated during radio-frequency magnetron sputtering of a hydroxyapatite target, appear to be a promising method of surface modification of bioresorbable polymer material (PCL) for tissue engineering.

A solution blow spinning technique is a method developed recently for making nonwoven webs of micro- and nanofibres. The principal advantage of this method compared to a more traditional electrospinning process is its significantly higher production rate. In this work, the solution blow spinning method was further developed to produce nonwoven polymeric scaffolds based on a copolymer of tetrafluoroethylene with vinylidene fluoride solution in acetone. A crucial feature of the proposed method is that high-voltage equipment is not required, which further improves the method's economics. Scanning electron microscopy analysis of the samples demonstrated that the surface morphology of the nonwoven materials is dependent on the polymer concentration in the spinning solution. It was concluded that an optimum morphology of the nonwoven scaffolds for medical applications is achieved by using a 5% solution of the copolymer. It was established that the scaffolds produced from the 5% solution have a fractal structure and anisotropic mechanical properties. X-ray diffraction, infrared spectroscopy, Raman spectroscopy and differential scanning calorimetry demonstrated that the fabricated nonwoven materials have crystal structures that exhibit ferroelectric properties. Gas chromatography has shown that the amount of acetone in the nonwoven material does not exceed the maximum allowable concentration of 0.5%. In vitro analysis, using the culture of motile cells, confirmed that the nonwoven material is non-toxic and does not alter the morpho-functional status of stem cells for short-term cultivation, and therefore can potentially be used in medical applications., (Copyright © 2014 Elsevier B.V. All rights reserved.)