Search Results (14)

This study aims to demonstrate the possibility of incorporating a natural antioxidant biomolecule into polymeric porous scaffolds. To this end, Poly-l-Lactic Acid (PLLA) scaffolds were produced using the Thermally Induced Phase Separation (TIPS) technique and additivated with different amounts of rosmarinic acid (RA). The scaffolds, with a diameter of 4 mm and a thickness of 2 mm, were characterized with a multi-analytical approach. Specifically, Scanning Electron Microscopy analyses demonstrated the presence of an interconnected porous network, characterized by a layer of RA at the level of the pore’s surfaces. Moreover, the presence of RA biomolecules increased the hydrophilic nature of the sample, as evidenced by the decrease in the contact angle with water from 128° to 76°. The structure of PLLA and PLLA containing RA molecules has been investigated through DSC and XRD analyses, and the obtained results suggest that the crystallinity decreases when increasing the RA content. This approach is cost-effective, and it can be customized with different biomolecules, offering the possibility of producing porous polymeric structures containing antioxidant molecules. These scaffolds meet the requirements of tissue engineering and could offer a potential solution to reduce inflammation associated with scaffold implantation, thus improving tissue regeneration. Full article

Ethylene-chlorotrifluoroethylene (ECTFE) was first commercialized by DuPont in 1974. Its unique chemical structure gives it high heat resistance, mechanical strength, and corrosion resistance. But also due to these properties, it is difficult to prepare a membrane from it by the nonsolvent-induced phase separation (NIPS) method. However, it can be prepared as a microfiltration membrane using the thermally induced phase separation (TIPS) method at certain temperatures and with the selection of suitable solvents, and the use of green solvents is receiving increasing attention from researchers. The surface wettability of ECTFE membranes usually needs to be modified before use to strengthen its performance to meet the application requirements, usually by graft modification and surface oxidation techniques. This paper provides an overview of the structure of ECTFE and its preparation and modification methods, as well as recent advances in its application areas and prospects for the future methods of preparing high-performance ECTFE membranes. Full article

The creation of multi-stimuli-sensitive composite polymer–inorganic materials is a practical scientific task. The combination of photoactive magneto-piezoelectric nanomaterials and ferroelectric polymers offers new properties that can help solve environmental and energy problems. Using the doctor blade casting method with the thermally induced phase separation (TIPS) technique, we synthesized a hybrid polymer–inorganic nanocomposite porous membrane based on polyvinylidene fluoride (PVDF) and bismuth ferrite (BiFeO₃/BFO). We studied the samples using transmission and scanning electron microscopy (TEM/SEM), infrared Fourier spectroscopy (FTIR), total transmission and diffuse reflection, fluorescence microscopy, photoluminescence (PL), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), vibrating-sample magnetometer (VSM), and piezopotential measurements. Our results demonstrate that the addition of BFO increases the proportion of the polar phase from 76.2% to 93.8% due to surface ion–dipole interaction. We also found that the sample exhibits laser-induced fluorescence, with maxima at 475 and 665 nm depending on the presence of nanoparticles in the polymer matrix. Furthermore, our piezo-photocatalytic experiments showed that under the combined actions of ultrasonic treatment and UV–visible light irradiation, the reaction rate increased by factors of 68, 13, 4.2, and 1.6 compared to sonolysis, photolysis, piezocatalysis, and photocatalysis, respectively. This behavior is explained by the piezoelectric potential and the narrowing of the band gap of the composite due to the mechanical stress caused by ultrasound. Full article

Bio-based and patient-specific three-dimensional (3D) scaffolds can present next generation strategies for bone tissue engineering (BTE) to treat critical bone size defects. In the present study, a composite filament of poly lactic acid (PLA) and 45S5 bioglass (BG) were used to 3D print scaffolds intended for bone tissue regeneration. The thermally induced phase separation (TIPS) technique was used to produce composite spheres that were extruded into a continuous filament to 3D print a variety of composite scaffolds. These scaffolds were analyzed for their macro- and microstructures, mechanical properties, in vitro cytotoxicity and in vivo biocompatibility. The results show that the BG particles were homogeneously distributed within the PLA matrix and contributed to an 80% increase in the mechanical strength of the scaffolds. The in vitro cytotoxicity analysis of PLA-BG scaffolds using L929 mouse fibroblast cells confirmed their biocompatibility. During the in vivo studies, the population of the cells showed an elevated level of macrophages and active fibroblasts that are involved in collagen extracellular matrix synthesis. This study demonstrates successful processing of PLA-BG 3D-printed composite scaffolds and their potential as an implant material with a tunable pore structure and mechanical properties for regenerative bone tissue engineering. Full article

In this research, we describe the properties of three-component composite foam scaffolds based on poly(ε-caprolactone) (PCL) as a matrix and hydroxyapatite whiskers (HAP) and L-Lysine as fillers (PCL/HAP/Lys with wt% ratio 50/48/2). The scaffolds were prepared using a thermally induced phase separation technique supported by salt leaching (TIPS-SL). All materials were precisely characterized: porosity, density, water uptake, wettability, DSC, and TGA measurements and compression tests were carried out. The microstructure of the obtained scaffolds was analyzed via SEM. It was found that the PCL/HAP/Lys scaffold has a 45% higher Young’s modulus and better wettability compared to the PCL/HAP system. At the same time, the porosity of the system was ~90%. The osteoblast hFOB 1.19 cell response was also investigated in osteogenic conditions (39 °C) and the cytokine release profile of interleukin (IL)-1β, IL-6, and tumor necrosis factor (TNF)-α was determined. Modification of PCL scaffolds with HAP and L-Lysine significantly improved the proliferation of pre-osteoblasts cultured on such materials. Full article

Polymeric scaffolds made of PCL/PLCL (ratio 1:3, respectively) blends have been developed by using the Thermally Induced Phase Separation (TIPS) process. A new additional technique has been introduced in this study by applying pre-heat treatment to the blend solution before the TIPS process. The main objective of this study is to evaluate the influence of the pre-heat treatment on mechanical properties. The mechanical evaluation showed that the mechanical strength of the scaffolds (including tensile strength, elastic modulus, and strain) improved as the temperature of the polymer blend solution increased. The effects on the microstructure features were also observed, such as increasing strut size and differences in phase separation morphology. Those microstructure changes due to temperature control contributed to the increasing of mechanical strength. The in vitro cell study showed that the PCL/PLCL blend scaffold exhibited better cytocompatibility than the neat PCL scaffold, indicated by a higher proliferation at 4 and 7 days in culture. This study highlighted that the improvement of the mechanical strength of polymer blends scaffolds can be achieved using a very versatile way by controlling the temperature of the polymer blend solution before the TIPS process. Full article

The fabrication of 3D scaffolds is under wide investigation in tissue engineering (TE) because of its incessant development of new advanced technologies and the improvement of traditional processes. Currently, scientific and clinical research focuses on scaffold characterization to restore the function of missing or damaged tissues. A key for suitable scaffold production is the guarantee of an interconnected porous structure that allows the cells to grow as in native tissue. The fabrication techniques should meet the appropriate requirements, including feasible reproducibility and time- and cost-effective assets. This is necessary for easy processability, which is associated with the large range of biomaterials supporting the use of fabrication technologies. This paper presents a review of scaffold fabrication methods starting from polymer solutions that provide highly porous structures under controlled process parameters. In this review, general information of solution-based technologies, including freeze-drying, thermally or diffusion induced phase separation (TIPS or DIPS), and electrospinning, are presented, along with an overview of their technological strategies and applications. Furthermore, the differences in the fabricated constructs in terms of pore size and distribution, porosity, morphology, and mechanical and biological properties, are clarified and critically reviewed. Then, the combination of these techniques for obtaining scaffolds is described, offering the advantages of mimicking the unique architecture of tissues and organs that are intrinsically difficult to design. Full article

In this research, we prepared foam scaffolds based on poly(l-lactide) (PLLA) and apatite whiskers (HAP) using thermally induced phase separation technique supported by the salt leaching process (TIPS-SL). Using sodium chloride having a size of (a) 150–315 μm, (b) 315–400 μm, and (c) 500–600 μm, three types of foams with different pore sizes have been obtained. Internal structure of the obtained materials has been investigated using SEM as well as μCT. The materials have been studied by means of porosity, density, and compression tests. As the most promising, the composite prepared with salt size of 500–600 μm was prepared also with the l-lysine modified apatite. The osteoblast hFOB 1.19 cell response for the scaffolds was also investigated by means of cell viability, proliferation, adhesion/penetration, and biomineralization. Direct contact cytotoxicity assay showed the cytocompatibility of the scaffolds. All types of foam scaffolds containing HAP whiskers, regardless the pore size or l-lysine modification induced significant stimulatory effect on the cal-cium deposits formation in osteoblasts. The PLLA/HAP scaffolds modified with l-lysine stimulated hFOB 1.19 osteoblasts proliferation. Compared to the scaffolds with smaller pores (150–315 µm and 315–400 µm), the PLLA/HAP foams with large pores (500–600 µm) promoted more effective ad-hesion of osteoblasts to the surface of the biomaterial. Full article

Porous biodegradable scaffolds provide a physical substrate for cells allowing them to attach, proliferate and guide the formation of new tissues. A variety of techniques have been developed to fabricate tissue engineering (TE) scaffolds, among them the most relevant is the thermally-induced phase separation (TIPS). This technique has been widely used in recent years to fabricate three-dimensional (3D) TE scaffolds. Low production cost, simple experimental procedure and easy processability together with the capability to produce highly porous scaffolds with controllable architecture justify the popularity of TIPS. This paper provides a general overview of the TIPS methodology applied for the preparation of 3D porous TE scaffolds. The recent advances in the fabrication of porous scaffolds through this technique, in terms of technology and material selection, have been reviewed. In addition, how properties can be effectively modified to serve as ideal substrates for specific target cells has been specifically addressed. Additionally, examples are offered with respect to changes of TIPS procedure parameters, the combination of TIPS with other techniques and innovations in polymer or filler selection. Full article

Human periapical cyst mesenchymal stem cells (hPCy-MSCs) are a newly discovered cell population innovatively collected from inflammatory periapical cysts. The use of this biological waste guarantees a source of stem cells without any impact on the surrounding healthy tissues, presenting a valuable potential in tissue engineering and regenerative medicine applications. In the present study, hPCy-MSCs were collected, isolated, and seeded on three experimental mineral-doped porous scaffolds produced by the thermally-induced phase-separation (TIPS) technique. Mineral-doped scaffolds, composed of polylactic acid (PLA), dicalcium phosphate dihydrate (DCPD), and/or hydraulic calcium silicate (CaSi), were produced by TIPS (PLA-10CaSi, PLA-5CaSi-5DCPD, PLA-10CaSi-10DCPD). Micro-CT analysis evaluated scaffolds micromorphology. Collected hPCy-MSCs, characterized by cytofluorimetry, were seeded on the scaffolds and tested for cell proliferation, cells viability, and gene expression for osteogenic and odontogenic differentiation (DMP-1, OSC, RUNX-2, HPRT). Micro-CT revealed an interconnected highly porous structure for all the scaffolds, similar total porosity with 99% open pores. Pore wall thickness increased with the percentage of CaSi and DCPD. Cells seeded on mineral-doped scaffolds showed a superior proliferation compared to pure PLA scaffolds (control), particularly on PLA-10CaSi-10DCPD at day 12. A higher number of non-viable (red stained) cells was observable on PLA scaffolds at days 14 and 21. DMP-1 expression increased in hPCy-MSCs cultured on all mineral-doped scaffolds, in particular on PLA-5CaSi-5DCPD and PLA-10CaSi-10DCPD. In conclusion, the innovative combination of experimental scaffolds colonized with autologous stem cells from periapical cyst represent a promising strategy for regenerative healing of periapical and alveolar bone. Full article

This work reports on the synthesis, with the thermally induced phase separation (TIPS) technique, of poly (l-lactide) (PLLA) scaffolds containing Fe-doped hydroxyapatite (FeHA) particles for bone regeneration. Magnetization curves and X-ray diffraction indicate two magnetic particle phases: FeHA and magnetite Fe₃O₄. Magnetic nanoparticles (MNPs) are approximately 30 ± 5 nm in width and 125 ± 25 nm in length, and show typical ferromagnetic properties, including coercivity and rapid saturation magnetization. Scanning electron microscopy (SEM) images of the magnetic scaffolds reveal their complex morphology changes with MNP concentration. Similarly, at compositions of approximately 20% MNPs, the phase separation changes, passing from solid–liquid to liquid–liquid as revealed by the hill-like structures, with low peaks that give the walls in the SEM images a surface pattern of micro-ruggedness typical of nucleation mechanisms and growth. In vitro degradation experiments, carried out for more than 28 weeks, demonstrated that the MNPs delay the scaffold degradation process. Cytotoxicity is appreciated for FeHA content above 20%. Full article

Thermally induced phase separation (TIPS) is a technique to prepare commercial membrane. However, the quick polymer crystallization during the quenching process will bring about a dense and thick skin layer and thus decrease permeability markedly. In this paper, a diluent mixture with upper critical solution temperature (UCST) was used to prepare polyvinylidene fluoride (PVDF) hollow fiber membrane. That is, the separation between diluent (propylene carbonate (PC)) and non-diluent (dioctyl terephthalate (DOTP)) occurred during the quenching process when the temperature of the dope was lower than 110 °C. The effects of separation between PC and DOTP and the resulting coalescence of DOTP on the PVDF crystallization process, microstructure, and the permeability of the membranes were analyzed. The results showed that the suitable PC/DOTP weight ratio reduced the thickness of the skin layer near the outer surface markedly and resulted in a porous outer surface, and the microstructure evolution process was proposed. The maximum pure water flux for the prepared membrane is up to 128.5 L·m⁻²·h⁻¹ even in a dry mode without using a hydrophilizing agent. The rejection rate of the carbonic particle is nearly 100%. This study presents a novel and simple way to fabricate the microporous membrane with the interconnected pore structure. Full article

In this paper we describe the synthesis of poly(ester ether urethane)s (PEEURs) by using selected raw materials to reach a biocompatible polyurethane (PU) for biomedical applications. PEEURs were synthesized by using aliphatic 1,6-hexamethylene diisocyanate (HDI), poly(ethylene glycol) (PEG), α,ω-dihydroxy(ethylene-butylene adipate) (Polios), 1,4-butanediol (BDO) as a chain extender and calcium glycerolphosphate salt (GPCa) as a modifier used to stimulate bone tissue regeneration. The obtained unmodified (PURs) and modified with GPCa (PURs-M) PEEURs were studied by various techniques. It was confirmed that urethane prepolymer reacts with GPCa modifier. Further analysis of the obtained PURs and PURs-M by Fourier transform infrared (FTIR) and Raman spectroscopy revealed the chemical composition typical for PUs by the confirmed presence of urethane bonds. Moreover, the FTIR and Raman spectra indicated that GPCa was incorporated into the main PU chain at least at one-side. The scanning electron microscopy (SEM) analysis of the PURs-M surface was in good agreement with the FTIR and Raman analysis due to the fact that inclusions were observed only at 20% of its surface, which were related to the non-reacted GPCa enclosed in the PUR matrix as filler. Further studies of hydrophilicity, mechanical properties, biocompatibility, short term-interactions, and calcification study lead to the final conclusion that the obtained PURs-M may by suitable candidate material for further scaffold fabrication. Scaffolds were prepared by the solvent casting/particulate leaching technique (SC/PL) combined with thermally-induced phase separation (TIPS). Such porous scaffolds had satisfactory pore sizes (36–100 μm) and porosity (77–82%) so as to be considered as suitable templates for bone tissue regeneration. Full article

In this work composite hollow-fibers were prepared by dip-coating of commercial polypropylene (PP) with a thin layer of ethylene–chlorotrifluoroethylene copolymer (ECTFE). The employment of N-methyl pyrrolidone (NMP) as solvent improved the polymer processability favoring dip-coating at lower temperature (135 °C). Scanning electron microscopy (SEM) analyses showed that after dip-coating the PP support maintained its microstructure, whereas a thin coated layer of ECTFE on the external surface of the PP hollow-fiber was clearly distinguishable. Membrane characterization evidenced the effects of the concentration of ECTFE in the dope-solution and the time of dip-coating on the thickness of ECTFE layer and membrane properties (i.e., contact angle and pore size). ECTFE coating decreased the surface roughness reducing, as a consequence, the hydrophobicity of the membrane. Moreover, increasing the ECTFE concentration and dip-coating time enabled the preparation of a thicker layer of ECTFE with low and narrow pore size that negatively affected the water transport. On the basis of the superior chemical resistance of ECTFE, ECTFE/PP composite hollow fibers could be considered as very promising candidates to be employed in membrane processes involving harsh conditions. Full article