In vitro degradation and bioactivity of composite poly-<Emphasis Type="SmallCaps">l</Emphasis>-lactic (PLLA)/bioactive glass (BG) scaffolds: comparison of 45S5 and 1393BG compositions

The objective of this study was to compare the effect of two bioglass (BG) compositions 45S5 and 1393 in poly-l-lactic composite scaffolds in terms of morphology, mechanical properties, biodegradation, water uptake and bioactivity. The scaffolds were produced via thermally induced phase separation starting from a ternary polymer solution (polymer/solvent/non-solvent). Furthermore, different BG to polymer ratios have been selected (1, 2.5, 5% wt/wt) to evaluate the effect of the amount of filler on the composite structure. Results show that the addition of 1393BG does not affect the scaffold morphology, whereas the 45S5BG at the highest amount tends to appreciably modify the scaffold architecture interacting with the phase separation process. Bioactivity tests confirmed the formation of a hydroxycarbonateapatite-layer in both types of BGs (detected via scanning electron microscopy, X-ray diffractometry and Fourier Transform Infrared Spectroscopy). Overall, the results showed that 1393BG composition affects the experimental preparation protocol to a minimal extent thus allowing a better control of the scaffold’s morphology compared to 45S5BG.     

Fabrication and characterization of silk fibroin/bioactive glass composite films

Composite films of silk fibroin (SF) with nano bioactive glass (NBG) were prepared by the solvent casting method, and the structures and properties of the composite films were characterized. Fourier transform infrared (FT-IR) spectroscopy analysis shows that the random coil and β-sheet structure co-exist in the SF films. Results of field emission scanning electron microscope (FESEM) indicate that the NBG particles are uniformly dispersed in the SF films. The measurements of the water contact angles suggest that the incorporation of NBG into SF can improve the hydrophilicity of the composites. The bioactivity of the composite films was evaluated by soaking in 1.5 times simulated body fluid (1.5 × SBF), and formation of a hydroxycarbonate apatite (HCA) layer was determined by XRD and FESEM. The results show that the SF/NBG composite film is bioactive as it induces the formation of HCA on the surface of the composite film after soaking in 1.5 × SBF for 7 days. In vitro osteoblasts attachment and proliferation tests show that the composite film is a good matrix for the growth of osteoblasts. Consequently, the incorporation of NBG into the SF film can enhance both the bioactivity and biocompatibility of the film, which suggests that the SF/NBG composite film may be a potential biomaterial for bone tissue engineering.     

Synthesis and in vitro bioactivity of mesoporous bioactive glass scaffolds

The main objective of the present study was to determine the effect of thermal treatment procedures (calcination temperature, heating rate and duration time) on the synthesis of SiO₂–CaO–P₂O₅ mesoporous bioactive glass scaffolds. This is accomplished by thermogravimetric analyses, Fourier transform infrared (FTIR) absorption spectra, X-ray diffraction (XRD) and by analysis of nitrogen adsorption/desorption isotherms. In vitro bioactivity can also be assessed by the cytotoxic effect of the glasses on the NIH-3T3 cell line, and by characterization of MC-3T3-E1 cell attachment.     

Fabrication of porous bioactive glass particles by one step sintering

In this study, we reported a facile method to prepare porous bioactive glass microparticles. Porous particles were synthesized by sintering hollow bioactive glass microspheres obtained using a sol-gel co-template technology. The results showed that porous bioactive glass particles possessed a narrow particle size distribution, a relatively porous surface morphology and a hollow structure. It is worth to say that the resulting microparticles present an amorphous structure although the sintering temperature was improved compared to hollow microspheres. The presence of macropore on the shell may provide an efficient method to carry drugs in the hollow cores. Considering the high deposit rate of nanoscale apatite for bioactive glass materials, the porous microparticles should have potential applications in drug and bioactive molecules delivery, in addition to bone tissue regeneration.     

Fabrication of ultra thin and aligned carbon nanofibres from electrospun polyacrylonitrile nanofibres

Ultra thin and aligned carbon nanofibres (CNFs) have been fabricated by heat treatment from aligned polyacrylonitrile (PAN) nanofibre precursors prepared by electrospinning. The alignment of the precursor nanofibres was achieved by using a modified electrospinning set up developed recently, where a tip collector was used to collect and align the nanofibres. The average diameter of the aligned CNFs is about 80 nm. The stabilization and carbonization behaviour were studied mainly based on the randomly oriented PAN nanofibres. The effects of stabilization and carbonization temperatures, temperature-increasing rates, and with and without substrates on the morphology and structure of the CNFs were investigated. Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction, transmission electron microscopy and Raman spectroscopy were used to characterize the structure of the CNFs and thermogravimetric/differential temperature analysis was used to evaluate the thermal behaviour of PAN nanofibres.     

Fabrication of nanofibrous macroporous scaffolds of poly(lactic acid) incorporating bioactive glass nanoparticles by camphene-assisted phase separation

Here we produced macroporous and nanofibrous scaffolds with bioactive nanocomposite composition, poly(lactic acid) (PLA) incorporating bioactive glass nanoparticles (BGnp) up to 30 wt%, targeting bone regeneration. In particular, the nanofibrous structure in the scaffolds was generated by using a bicyclic monoterpene, camphene (C₁₀H₁₆), through a phase-separation process with PLA-BGnp phase in chloroform/1,4-dioxane co-solvent. Furthermore, macropores were produced by the impregnation of salt particles and their subsequent leaching out, followed by freezing and lyophilization processes. The produced PLA-BGnp scaffolds presented highly porous and nanofibrous structure with porosities of 90–95% and pore sizes of over hundreds of micrometers. BGnp with sizes of ∼90 nm were also evenly impregnated within the PLA matrix, featuring a nanocomposite structure. The nanofibrous scaffolds exhibited enhanced hydrophilicity and more rapid hydrolytic degradation as the incorporated BGnp content increased. The bone-bioactivity of the scaffolds was substantially improved with the incorporation of BGnp, exhibiting rapid formation of apatite throughout the scaffolds in a simulated body fluid. The developed macroporous and nanofibrous scaffolds with PLA-BGnp bioactive composition are considered as a novel 3D matrix potentially useful for bone tissue engineering.     

Synthesis and in vitro bioactivity of novel mesoporous hollow bioactive glass microspheres

The remarkable tissue-repairing bioactivity and biocompatibility of bioactive glass make it suitable for a wide range of applications. Here, novel mesoporous hollow bioactive glass microspheres (MHBGMs) with a uniform diameter range of 2-5 µm were prepared by a sol-gel method. Structural characterization indicated that the shell of hollow sphere had a mesopore size range between 2 and 10 nm and a thickness about 500 nm. The in vitro bioactivity test indicated that the novel structure exhibited high in vitro bioactivity. The uniform microspherical morphology and mesoporous hollow structure of MHBGMs, together with their high bioactivity, turn them into a good candidate as an injectable and drug-loading biomaterial for in vivo tissue regeneration and drug control release.     

Design of bioactive bone substitutes based on biomineralization process

A material able to form bone-like apatite on its surface in the living body bonds to living bone through the apatite layer. Functional groups such as Si-OH, Ti-OH, Zr-OH, Nb-OH and Ta-OH induce apatite formation in the living body. On the basis of these findings, various kinds of bioactive materials with different mechanical properties can be designed. For example, bioactive titanium metal, its alloys and tantalum metal can be obtained by forming a thin sodium titanate or tantalate layer on their surfaces by NaOH solution and heat treatments.Bioactive organic polymers can be obtained by forming a thin CaO–SiO₂ or TiO₂ layer on their surfaces by a sol–gel method. These bioactive materials are believed to be useful as unique bone substitutes.     

Fabrication and characterization of bioactive glass coatings produced by the ion beam sputter deposition technique

Ion beam sputtering and ion beam sputtering/mixing deposition techniques were used to produce thin bioactive glass coatings on titanium substrate. It was found that as-deposited coatings were amorphous. Scanning electron microscopical examination showed that the coatings had a uniform and dense structure and that fabrication parameters affected the surface morphology of the coatings. The surface Ca/P ratio of the coatings, which varied from 5.9 to 8.6 according to semi-quantitative EDX analyses, was correlated with the fabrication condition. Depth profiling of the coatings revealed four distinct zones: the top surface, the thin coating zone, the intermixed zone of coating and substrate, and the substrate. Scratch tests showed that the coatings adhered well to the substrate.     

Fabrication of hierarchical ZnO architectures by a biomineralization process

In this paper, hierarchical structured ZnO particles were successfully synthesized via a facile biomineralization process with the template of histidine at room temperature. Detailed microstructural characterization had been carried out using X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Role of histidine concentration in the hierarchical ZnO syntheses, including flower-type structure and mineral configuration, had been systematically investigated. Zn²⁺–histidine interaction was suggested to be the dominant growth factor. The room-temperature Raman spectrum of ZnO flower type revealed good crystal quality and increased Raman scattering. The PL spectrum of ZnO mineral structure showed stronger emission in a wide range of wavelengths.     

Fabrication and characterisation of polypropylene nanofibres by meltblowing process using different fluids

In nonwoven industry, meltblowing has been widely used as an important technique for the production of nonwoven webs consisting of microfibres, suitable for various applications. Recently, great attention is being paid to fabricate nonwoven webs consisting of nanofibres, commonly known as nanowebs. In this paper, polypropylene has been successfully used for the fabrication of nanowebs by meltblowing process with the injection of different fluids (such as air and water) at the vent port of commercial meltblowing equipment. The lowest average fibre diameters achieved were 755 and 438 nm by the use of air and water, respectively. Differential scanning calorimetry results showed the presence of single melting peaks in the first heating cycle and double melting peaks in the second, due to the re-crystallisation and re-organisation by heating during the experiments. The results obtained from thermo gravimetric analysis and intrinsic viscosity studies showed thermal degradation of the nanofibres during meltblowing. X-ray diffraction studies showed that all the meltblown polypropylene fibres produced with the injection of the fluids contained low degrees of crystallinity and monoclinic α-form crystals. The crystallinity was increased with annealing. Similar Fourier transform infrared spectra of the polymer and the fibres indicated no change to the chemical functionality of the nanofibres by the application of the fluids and high temperature during meltblowing.     

Facile synthesis and in vitro bioactivity of radial mesoporous bioactive glass with high phosphorus and calcium content

A novel uniform monodispersed radial mesoporous bioactive glass nanosphere (MBG) with high phosphorus and calcium content has been successfully synthesized. The synthesis was first taken place in a cyclohexane-water biphasic stratification reaction system, which fabricated the radial mesoporous SiO₂-P₂O₅ nanosphere (SPN) using hexadecyltrimethyl ammonium bromide (CTAB) as a template agent and triethanolamine (TEA) as a hydrolysis catalyst. Solid reactions were then carried out to synthesize SiO₂-CaO-P₂O₅ MBG using SPN as both the silicon source and phosphorus source, and Ca(NO₃)₂ as the calcium source. The prepared MBG not only displayed the radial structure and high specific surface area (~321 m²/g), but also had high phosphorus and calcium content. The results of energy dispersive spectrometer (EDS) demonstrated that P₂O₅ content was enhanced by properly increasing the reaction temperature. The in vitro bioactivity test showed that MBG had an excellent ability of inducing apatite formation. Furthermore, the MBG showed excellent biocompatibility at a low concentration of 50–100 μg/mL in vitro, and it would have a promising prospect as drug delivery system for bone tissue regeneration.     

Comparison in in-vivo response between a bioactive glass and a non-bioactive glass

The authors report on the in-vivo comparison, in the rabbit, between the response to a bioactive glass and the response to a non-bioactive glass. Implants have been performed in muscle and bone. Two different glasses were investigated, namely B01 and I02. B01 is a glass designed to be degradable and resorbable and has a percentual molar composition of: 47.7% with a 1 : 1 CaO/Na₂O ratio. I02 is a sodium-calcium-silicate non-resorbable glass lacking P₂O₅ and has a percentual molar composition of: 29.3%. In-vivo tests were planned as: (a) intramuscular implants of glass cylinders in the rectus femoris and retrievals took place at 2, 16 and 43 weeks; (b) intraosseus implants of glass cylinders in the distal femural canal and retrievals took place at 8 and 43 weeks. Histology and light microscopy analysis followed. Bioactive degradable glass elicits a favorable response both in muscle and bone; a gradual degradation process leads to disruption and partial resorption of the material and a tight apposition is promoted with the newly formed bone. The non-bioactive sodium-calcium-silicate glass (named I02) may elicit, like the bioactive degradable B01, a favorable response which is characterized by the absence of inflammatory or other adverse reactions; anyway it does not change its structure at an optical microscopic level and it does not promote any tight apposition with bone. ©2000 Kluwer Academic Publishers     

Composite nanofiber of bioactive glass nanofiller incorporated poly(lactic acid) for bone regeneration

A novel composite nanofiber of poly(lactic acid) (PLA) incorporated with the nanocomponent of bioactive glass was exploited using an electrospinning method. Small concentrations of the bioactive glass phase added up to 10% facilitated the generation of a nanofibrous matrix with hundreds of nanometers in diameter without a formation of beads. The addition of the bioactive glass phase greatly enhanced the in vitro apatite formation on the nanofiber surface under a body simulating medium. Osteoblastic cells were demonstrated to adhere well on the composite nanofiber and grow actively with culturing time, suggesting its usefulness as a supporting matrix for the hard tissue regeneration.     

Effect of nanoparticulate bioactive glass particles on bioactivity and cytocompatibility of poly(3-hydroxybutyrate) composites

This work investigated the effect of adding nanoparticulate (29 nm) bioactive glass particles on the bioactivity, degradation and in vitro cytocompatibility of poly(3-hydroxybutyrate) (P(3HB)) composites/nano-sized bioactive glass (n-BG). Two different concentrations (10 and 20 wt %) of nanoscale bioactive glass particles of 45S5 Bioglass composition were used to prepare composite films. Several techniques (Raman spectroscopy, scanning electron microscopy, atomic force microscopy, energy dispersive X-ray) were used to monitor their surface and bioreactivity over a 45-day period of immersion in simulated body fluid (SBF). All results suggested the P(3HB)/n-BG composites to be highly bioactive, confirmed by the formation of hydroxyapatite on material surfaces upon immersion in SBF. The weight loss and water uptake were found to increase on increasing bioactive glass content. Cytocompatibility study (cell proliferation, cell attachment, alkaline phosphatase activity and osteocalcin production) using human MG-63 osteoblast-like cells in osteogenic and non-osteogenic medium showed that the composite substrates are suitable for cell attachment, proliferation and differentiation.     

Fabrication of 3-D gelatin-patterned glass substrates with layer-by-layer and lift-off (LbL-LO) technology

The assembly of multilayer films of gelatin onto glass substrates using layer-by-layer and lift-off (LbL-LO) technology to modify the surface topography and chemistry properties of in vitro cell culture scaffolds is described. The ability to generate such nanoscale systems containing cell-adhesive materials on optically transparent substrates with microscale lateral dimensions, nanoscale vertical dimensions, molecular vertical precision, and flexibility in material selection has important implications for tissue engineering, drug discovery, and basic research in cell biology. Toward this goal, a systematic study on the electrostatic adsorption properties of fluorescein 5-isothiocyanate-gelatin B (FITC-gelatin) was completed. In addition, the integration of protein nanoassembly with microlithographic feature definition was used to pattern three-dimensional FITC-gelatin nanofilms on planar glass substrates. The experimental results indicate that FITC-gelatin is negatively charged at pH 9 and can be alternately assembled with a positively charged polyion, poly(diallyldimethylammonium chloride) (PDDA), to form multilayer films on solid templates with thickness of 5-10 nm per bilayer. Furthermore, images of protein/polymer nanocomposites indicate that LbL-LO is an efficient way to realize the designed substrates. These findings will benefit future research on cell culture and tissue engineering that require methods of generating protein patterns to fabricate novel in vitro cell culture systems.     

Structure and crystallization behavior of borate-based bioactive glass

The structure and crystallization behavior of borate-based bioactive glass, designated 45S5B1, were investigated by Fourier transform infrared (FTIR) spectroscopy, differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). FTIR spectroscopy revealed that the network structure of the glass consisted mainly of [BO₃], [BO₄] and [PO₄] units. Two distinct crystallization peaks were observed for this glass by DTA, with activation energies of 475 and 210 kJ/mol, respectively. XRD indicated that the crystallization process with higher activation was associated with the formation of CaNa₃B₅O₁₀, whereas the process with the lower activation energy was associated with the formation of CaB₂O₄. The results indicated that the crystallization process in 45S5B1 glass was dominated by bulk crystallization, although surface crystallization also occurred for small particle sizes (<50 μm).     

含锶硼酸盐基生物玻璃经晶化处理后对其溶解性能及体外生物活性的影响

通过对含锶硼酸盐基玻璃进行微晶化处理,以考察该玻璃由玻璃态转化为晶态时体外生物活性和降解性的改变。采用熔融法制备不同锶含量(n(SrO)=0、2%、6%)的硼硅酸盐生物玻璃,然后在700℃/4h条件下微晶化处理,分别获得微晶化前后的试样。将各组玻璃及微晶化的样品浸泡在类似于生理模拟液的0.02mol/L的K2HPO4溶液中(以1g玻璃对应100mL浸泡液的比例),置于37℃恒温条件下,进行体外生物矿化反应。用XRD和FT-IR对反应后产物进行表征,并测定不同浸泡时间下样品的质量损失率以及浸泡液的pH值。结果表明,微晶化处理前后的含锶的硼硅酸盐玻璃试样在浸泡实验中都可以转化成含锶羟基磷灰石,即微晶化后的试样仍然具有体外生物活性;并且微晶化后试样的离子溶出速度能够减缓,降低了原玻璃相对骨组织生长来说的较高的降解速度,可以更加匹配骨组织生长的周期。因此,微晶化处理硼硅酸盐玻璃可实现对降解速度的调控,使该微晶化的生物玻璃有可能在骨组织修复中得到临床应用。     

Fabrication of highly oriented (002) ZnO film on glass by sol-gel method

In this study high quality (002) ZnO films were deposited on glass substrate by a sol-gel spin coating process. The as-coated films were post-annealed at different temperatures in air to investigate the effect of annealing temperature in particular. The chemical composition of the precursor sol and the intermediates produced in the films heating process were analyzed by thermo gravimetric analysis/differential thermal analysis (TGA/DTA). The microstructure and its optical properties of ZnO films were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), ultraviolet-visible spectroscopy (UV-Vis) and photoluminescence. TGA/DTA showed that a significant weight loss occurred at around 200-300 °C and the weight stabilized at 300 °C. An extremely sharp (002) diffracted peak in XRD patterns indicated the high preference in crystallinity of these films. FESEM micrographs revealed that the films were filled with particulates with size ranging from 10 to 25 nm as post annealing temperature increased from 400 to 500 °C and turned into porous films at 600 °C. UV-Vis has shown that the films were highly transparent under visible light and had a sharp absorption edge in the ultraviolet region at 380 nm. The measured optical band gap values of the ZnO thin films were around 3.24-3.26 eV. Photoluminescence spectra revealed a strong UV emission centered at about 390 nm corresponding to the near-band-edge emission with a weak defect-related emission at about 520 nm. The intensity of UV emission increased with the annealing temperature. This may be attributed to a higher quality ZnO film while annealed at higher temperature.     

In vitro evaluation of borate-based bioactive glass scaffolds prepared by a polymer foam replication method

Borate-based bioactive glass scaffolds with a microstructure similar to that of human trabecular bone were prepared using a polymer foam replication method, and evaluated in vitro for potential bone repair applications. The scaffolds (porosity = 72 ± 3%; pore size = 250–500 μm) had a compressive strength of 6.4 ± 1.0 MPa. The bioactivity of the scaffolds was confirmed by the formation of a hydroxyapatite (HA) layer on the surface of the glass within 7 days in 0.02 M K₂HPO₄ solution at 37 °C. The biocompatibility of the scaffolds was assessed from the response of cells to extracts of the dissolution products of the scaffolds, using assays of MTT hydrolysis, cell viability, and alkaline phosphatase activity. For boron concentrations below a threshold value (0.65 mM), extracts of the glass dissolution products supported the proliferation of bone marrow stromal cells, as well as the proliferation and function of murine MLO-A5 cells, an osteogenic cell line. Scanning electron microscopy showed attachment and continuous increase in the density of MLO-A5 cells cultured on the surface of the glass scaffolds. The results indicate that borate-based bioactive glass could be a potential scaffold material for bone tissue engineering provided that the boron released from the glass could be controlled below a threshold value.