Bioactive glass induced in vitro apatite formation on composite GBR membranes.

The aim of this study was to investigate in vitro bioactivity of different thermoplastic biodegradable barrier membranes. Three experimental GBR membranes were fabricated using Poly(epsilon-caprolactone-co-D: ,L-lactide) P(CL/DL-LA) and particulate bioactive glass S53P4 (BAG; granule size 90-315 microm): (A) composite membrane with 60-wt.% of BAG, (B) membrane coated with BAG; and (C) copolymer membrane without BAG. Membranes were immersed in simulated body fluid (SBF), and their surfaces were characterized with SEM, XRD and EDS after 6 and 12 h and after 1, 3, 5, 7, and 14 days. Calcium phosphate (Ca-P) surface formation was observed on both composite membranes (A and B) but not on the copolymer membrane without bioactive glass (C). The Ca-P precipitation appeared to be initiated on the bioactive glass followed by growth of the layer along the polymer surface. In 6-12 h ion dissolution of the bioactive glass led to formation of the silica rich layer on the surface of the exposed glass granules on composite membrane B whereas only small amounts of silica was observed on the polymer surface of the composite membrane A. At 24 h nucleation of Ca-P precipitation was observed, and by 3-5 days membrane surface was covered with a uniform Ca-P layer transforming from amorphous to low crystalline structure. At 7 days composition and structure of the apatite surface resembled the apatite in bone. Once nucleated, the surface topography seemed to have significant effect on the growth of the apatite layer.

Bioactive glass S53P4 in frontal sinus obliteration: a long-term clinical experience.

BACKGROUND: Synthetic, osteoconductive, and antimicrobial bioactive glass (BAG) has been used in many surgical applications. METHODS: BAG was used as obliteration material in a series of osteoplastic frontal sinus operations on 42 patients suffering from chronic frontal sinusitis, which could not be cured with other means of treatment. RESULTS: Accurate obliteration of sinuses was achieved in 39 patients. Uneventful recovery and clinical outcome were seen in 92% of the patients. Histopathologic samples harvested at 1, 5, and 10 years after obliteration revealed a healing process progressing from the fibrous tissue phase to bone formation with scattered fibrous tissue and bony obliteration maintaining BAG granule remnants. Fourier-transform infrared (FTIR) studies showed bone produced by BAG to be similar to natural frontal bone. Micorobiologic cultures obtained with histologic samples revealed no growth of bacteria. CONCLUSIONS: BAG appears to be a reliable frontal sinus obliteration material, providing favorable conditions for total bony sinus obliteration.

Exothermal characteristics and release of residual monomers from fiber-reinforced oligomer-modified acrylic bone cement.

The aim of this study is to determine the peak temperature of polymerization, the setting time and the release of residual monomers of a modified acrylic bone cement. Palacos R, a commercial bone cement, is used as the main component. The cement is modified by adding short glass fibers and resorbable oligomer fillers, and an additional cross-linking monomer. The test specimens are classified according to the composition of the bone cement matrix (i.e., oligomer-filler, glass-fiber reinforcement, and/or cross-linking monomer). The exothermal characteristics during autopolymerization are analyzed using a transducer connected with a computer. The quantities of residual monomers were analyzed from different test groups using high performance liquid chromatography (HPLC). The DeltaT value for the oligomer filler and the glass-fiber-containing acrylic bone cement is lower than that for the unmodified bone cement (2.1 +/- 0.8 vs. 23.5 +/- 4.2 degrees C). The addition of a cross-linking monomer, EGDMA, shortens the setting time of the autopolymerization of the unmodified bone cement (7.1 +/- 0.9 min vs. 3.3 +/- 0.3 min). The quantity of the residual monomers released is higher in the modified bone cement than that in the unmodified cement. The cement that contains glass fibers and oligomer fillers has a considerably lower exothermal peak, whereas the total quantity of residual monomers released is increased.

Synthesis and characterization of polyamide of trans-4-hydroxy-L-proline used as porogen filler in acrylic bone cement.

The aim of this study was to synthesize on a larger scale, an experimental polyamide based on an amino acid of trans-4-hydroxy-L-proline. The polyamide of trans-4-hydroxy-L-proline has been used as porogen filler (i.e., a hydrophilic pore generating material) in nondegradable acrylic bone cement. In in vitro studies, this hydrophilic filling component has been shown to form porosity within the acrylic bone cement in an aqueous environment. The formation of in situ porosity in the acrylic polymer matrix is believed to improve the fixation between the cement and the living bone. Namely, a porous structure can support bone ingrowth and strengthen the mechanical connection between the acrylic bone cement and the bone. The monomer, trans-4-hydroxy-L-proline methyl ester, was prepared from trans-4-hydroxy-L-proline by means of two steps, and the monomer was then polymerized to polyamide of trans-4-hydroxy-L-proline. The polymerization was carried out using a melt polycondensation method. The molecular weights (M(psi)) of the produced polyamides were between 1800 and 3600. The products were characterized by FTIR and (1)H-NMR spectroscopy.

Shear bond strength of Bis-GMA resin and methacrylated dendrimer resins on silanized titanium substrate.

OBJECTIVES: The study compared the bond strengths of three resins, Bis-GMA and two novel experimental methacrylated polyester dendrimer resins to grit-blasted titanium substrate with three silanes. METHODS: Two commercial dental silanes (ESPE Sil and Monobond-S) and an experimental 0.5 vol% 3-methacryloxypropyltrimethoxysilane were applied to grit-blasted Ti substrates. Light-polymerizable resins of Bis-GMA and methacrylated dendrimer were applied to the grit-blasted Ti substrate with polyethylene molds. The substrates with resin stubs (n = 10) were thermocycled (6000 cycles, 5-55 degrees C) or kept in water (37 degrees C, 24 h). The shear bond strength of the resin was measured at a crosshead speed of 1.0 mm min(-1). The surface examination, before and after silanization, was made with a scanning electron microscope (SEM). The silane reactions on the Ti surface were monitored by Fourier transform infrared spectrometry. RESULTS: Statistical analysis (ANOVA) showed that the highest shear bond for thermocycled samples was obtained for Bis-GMA with Monobond-S (19.4 MPa, standard deviation (SD) 7.1 MPa), and after water storage with a laboratory-made silane (26.4 MPa, SD 8.1 MPa). The dendrimer and Bis-GMA resins conferred equal bonding properties to grit-blasted titanium after thermocycling. The silane, resin type, and storage conditions significantly affected the shear bond strength (p < 0.001 for all factors). SEM images suggested a mainly cohesive type of bonding failure. SIGNIFICANCE: A dendrimer based resin and the Bis-GMA resin systems conferred statistically equivalent bonding properties to silica-coated Ti after thermocycling.

Hydroxyapatite coating of cellulose sponge does not improve its osteogenic potency in rat bone.

Regenerated cellulose sponges were coated biomimetically with hydroxyapatite to increase their osteogenic properties. Induction of apatite precipitation was carried out with bioactive glass in simulated body fluid (SBF) for 24 h and the final coating was carried out in 1.5 x concentrated SBF for 14 days. Biomimetically mineralized and non-mineralized sponges were then implanted into standard size femoral cortical defects of rats, and the invasion of bone into the implant was followed up to one year. The apatite coating did not improve the osteoconductive property of cellulose in this rat cortical defect model. In fact, it generated a strong and highly cellular inflammatory reaction and less osteoid tissue. The biomimetic implants contained more immunodetectable TGFbeta1 (a strong stimulator of fibroblast activity) than untreated implants, and also bound more TGFbeta1 in vitro, which could, at least in part, explain the fibrotic invasion of biomimetically mineralized sponges.

Injectable bioactive glass/biodegradable polymer composite for bone and cartilage reconstruction: concept and experimental outcome with thermoplastic composites of poly(epsilon-caprolactone-co-D,L-lactide) and bioactive glass S53P4.

Injectable composites (Glepron) of particulate bioactive glass S53P4 (BAG) and Poly(epsilon-caprolactone-co-D,L-lactide) as thermoplastic carrier matrix were investigated as bone fillers in cancellous and cartilagineous subchondral bone defects in rabbits. Composites were injected as viscous liquid or mouldable paste. The glass granules of the composites resulted in good osteoconductivity and bone bonding that occurred initially at the interface between the glass and the host bone. The bone bioactivity index (BBI) indicating bone contacts between BAG and bone, as well as the bone coverage index (BCI) indicating bone ongrowth, correlated with the amount of glass in the composites. The indices were highest with 70 wt % of BAG, granule size 90-315 microm and did not improve by the addition of sucrose as in situ porosity creating agent in the composite or by using smaller (<45 microm) glass granules. The percentage of new bone ingrowth into the composite with 70 wt % of BAG was 6-8% at 23 weeks. At the articular surface cartilage regeneration with chondroblasts and mature chondrocytes was often evident. The composites were osteoconductive and easy to handle with short setting time. They were biocompatible with low foreign body cellular reaction. Results indicate a suitable working concept as a filler bone substitute for subchondral cancellous bone defects.

Flexural properties of crosslinked and oligomer-modified glass-fibre reinforced acrylic bone cement.

The flexural properties of oligomer-modified bone cement with various quantities of crosslinking monomer with or without glass fibre reinforcement were studied. The flexural strength and modulus of acrylic bone cement-based test specimens (N=6), including crosslinked and oligomer-modified structures with or without glass fibres, were measured in dry conditions and after immersion in simulated body fluid (SBF) for seven days (analysis with ANOVA). One test specimen from the acrylic bone cement group containing 30 wt % crosslinking monomer of its total monomer content was examined with scanning electron microscope (SEM) to evaluate signs of the semi-interpenetrating polymer network (semi-IPN). The highest dry mean flexural strength (130 MPa) was achieved with the bone cement/crosslinking monomer/glass fibre combination containing 5 wt % crosslinking monomer of its monomer content. The highest flexural modulus (11.5 GPa) was achieved with the bone cement/crosslinking monomer/glass fibre combination containing 30 wt % crosslinking monomer of its monomer content. SBF storage decreased the flexural properties of the test specimens, as did the addition of the oligomer filler. Nevertheless, the addition of crosslinking monomer and chopped glass fibres improves considerably the mechanical properties of oligomer-modified (i.e. porosity-producing filler containing) acrylic bone cement. In addition, some signs of the semi-IPN structure were observed by SEM examination.

An introduction to silanes and their clinical applications in dentistry.

PURPOSE: This overview presents a description of organofunctional trialkoxysilane coupling agents (silanes), their chemistry, properties, use, and some of the main clinical experiences in dentistry. MATERIALS AND METHODS: The main emphasis was on major dental journals that have been reviewed from 1958 up to the latest research news from 2002. A MEDLINE search with the key words "dental silanes" was used. Special silane literature and journals outside dentistry were also cited. RESULTS: The main emphasis is on the use of silanes in prosthetic and restorative dentistry. Clinical relevance was based mainly on either short- or long-term tests. The interpretation of various results is not given, mainly because of controversial observations that may be very difficult to explain. Nevertheless, the majority of the clinical results pointed to silanes playing a significant role in the adhesion process. Silane reaction mechanisms were not entirely understood, and there exist several theories for bonding mechanisms for silanes and substrates. CONCLUSION: Dental materials offer a continuously challenging forum for silanes, and silanes will play an essential role in material development.

Repair bond strength of restorative resin composite applied to fiber-reinforced composite substrate.

Delamination or fracture of composite veneers can occur as a result of improper design of the fiber-reinforced composite (FRC) framework. This in vitro study tested the repair bond strength of restorative composite to aged FRC. The substrate was multiphase polymer matrix FRC (everStick) aged by boiling for 8 h and storing at 37 degrees C in water for 6 weeks. The aged substrate surfaces were wet-ground flat with 1200-grit silicon carbide paper and subjected randomly to 5 different surface treatments: 1) An adhesion primer (Composite Activator) and resin (CA), 2) Silane (EspeSil) and resin (SIL-MP), 3) Silane, adhesive primer, and resin (Clearfil Repair) (CF), 4) Air particle-abrading (CoJet), silane, and resin (CJ-SIL-MP), 5) Resin (Scotchbond Multipurpose Resin) only as control (MP). Restorative composite resin (Z250) was added to the substrate in 2 mm layer increments and light-cured. Subsequently, every surface treatment group was divided into 2 subgroups of 12 specimens each. The specimens were either 48 h water-stored or thermocycled (6000 x 5-55 degrees C). The shear bond strengths of composite resin to FRC were measured at a crosshead speed of 1.0 mm/min. The data were analyzed by ANOVA for factors 'treatment type' and 'storage condition'; Tukey's post-hoc tests and Weibull analysis were performed. ANOVA showed a significant difference as a function of surface treatment (P<0.05) and storage condition (P<0.05). The CJ-SIL-MP group showed highest bond strength and Weibull modulus after thermocycling. Repair of multiphase polymer matrix FRC may show reliable bond strength when silane treatment is used along with air-particle abrading.

Bioactive glass granules as a bone adjunctive material in maxillary sinus floor augmentation.

OBJECTIVES: Bilateral sinus floor augmentation procedure was performed in 17 patients to study the effect of bioactive glass (BG) granules mixed with autologous bone (AB) chips on bone regeneration. The posterior part of 17 maxillary sinus was augmented with a 1:1 mixture of BG granules (phi 800-1000 microm) and AB chips harvested from the iliac crest (BG-AB group). The anterior parts of the same sinus and the contralateral sinus, serving as a control (AB group), were filled with AB chips alone. Trephine biopsies for histological, scanning electron microscopy (SEM), and energy dispersive X-ray (EDX) analyses were taken from the posterior part of the sinus after 21-34 weeks at the time of insertion of dental implants. Additionally, six biopsies were taken from the BG-AB group and four biopsies were taken from the AB group in connection with abutment operation at 49-62 weeks. RESULTS: Histological evaluation revealed lamellar bone growth in all the specimens. Although most of the BG granules were without bone contact in the majority of the patients in the BG-AB group, the bone lamellae were thicker than observed in the AB group. In the contact areas, bone was growing along the glass surface connecting the particles together. Histomorphometrical analysis carried out from the SEM images at 21-34 weeks revealed 26% and 25% bone in the BG-AB and the AB group, respectively. Corresponding figures for 49-62 weeks were 29% for the BG-AB group and 25% for the AB group. Bone-BG complex, i.e. the granules with intimate contact with bone, occupied 34% of the area measured at 21-34 weeks and 31% at 49-62 weeks. EDX analysis showed a tight contact and chemical bonding between the glass and bone. As a sign of dissolution, a few small Si-depleted areas were present in some BG granules at 21-34 weeks, while more and larger Si-free areas were observed in the granules at 49-62 weeks. CONCLUSION: The results indicate that BG granules (S53P4) can be used together with AB chips for sinus floor augmentation procedure, thus decreasing the amount of bone needed. Further studies concerning especially the biomechanical properties of the BG-AB complex with dental implants are needed.

Calcium phosphate formation and ion dissolution rates in silica gel-PDLLA composites.

Sol-gel derived silicas are potential biomaterials both for tissue regeneration and drug delivery applications. In this study, both SiO(2) and calcium and phosphate-containing SiO(2) (CaPSiO(2)) are combined with poly-(DL-lactide) to form a composite. The main properties studied are the ion release rates of biologically important ions (soluble SiO(2) and Ca(2+)) and the formation of bone mineral-like calcium phosphate (CaP) on the composite surface. These properties are studied by varying the quality, content and granule size of silica gel in the composite, and porosity of the polymer. The results indicate that release rates of SiO(2) and Ca(2+) depend mostly on the formed CaP layer, but in some extent also on the granule size of silicas and polymer porosity. The formation of the bone mineral-like CaP is suggested to be induced by a thin SiO(-) layer on the composite surface. However, due to absence of active SiO(2) or CaPSiO(2) granules on the outermost surface, the suitable nanoscale dimensions do not contribute the nucleation and growth and an extra source for calcium is needed instead. The result show also that all composites with varying amount of CaPSiO(2) (10-60 wt%) formed bone mineral-like CaP on their surfaces, which provides possibilities to optimise the mechanical properties of composites.

Frontal sinus and skull bone defect obliteration with three synthetic bioactive materials. A comparative study.

Three synthetic bioactive materials were studied in an experimental model to compare their usability in a frontal sinus and a skull bone defect obliteration. Bioactive glass number 9 (BAG(1)), bioactive glass number 13 (BAG(2)), and hydroxyapatite (HA) granules were investigated. BAG(1) and HA granules have been previously tested clinically. The clinical usefulness of BAG(2) granules has not been tested. Upper bony walls of 45 Elco rabbits' frontal sinuses were drilled open from four separate holes with the use of a standard method. The skull bone defects and the sinuses in frontal bone were filled with BAG(1) or BAG(2) on one side, and with HA on the other side. Two parallel posterior defects were covered with a pedicled periosteum flap, and two anterior defects with a free flap. The resorption of materials, new bone, and fibrous-tissue formation were observed with a histomorphometric method at 1, 3, and 6 months postoperatively. Scanning-electron microscopy (SEM) and Fourier-transform infrared spectroscopy (FTIR) were done at 6 months. In histomorphometry, the new bone formation increased with all the investigated materials throughout the study (p < 0.001), but the results showed higher new bone formation in the defects filled with BAG(1) than in corresponding BAG(2)- or HA- filled defects. New bone formation and resorption of materials were faster in defects covered by pedicled than by free periosteum flaps (p < 0.001). Intimate contact between the used materials and new bone was confirmed by SEM. FTIR analysis of bone produced by BAG(1) and BAG(2) was of the same type as natural frontal bone. BAG(2) can be manufactured in various shapes, and thus, could possibly be used in clinical conditions requiring a special anatomical implant shape. However, more research is needed regarding this property of BAG(2).

Bone response to degradable thermoplastic composite in rabbits.

The aim of this study was to evaluate biologic behavior of a composite of bioactive glass (BAG) (S53P4) and copolymer of poly(epsilon-caprolactone-co-DL-lactide) in experimental bone defects in rabbits. Twenty New Zealand white rabbits were used for the study. Bone defects (4 x 6mm) were prepared in the medial surfaces of the femoral condyles and the tibia. Cavities were filled with three different composites: composite with 60 wt% of small BAG granules (granule size <45 microm) and composites with 40 and 60 wt% of large BAG granules (granule size 90-315 microm). Copolymer without BAG was used as a reference material. Follow-up period was 8 and 16 weeks. In the femur at 8 weeks all the samples were partly surrounded by fibrous capsule. New bone formation was noticed in the areas where glass granules were in direct contact with the bone. At 16 weeks fibrous capsule was thinner in all samples. Bone ingrowth was found in the superficial layers of the composites with large glass granules. However, the percent of direct bone contact decreased between 8 and 16 weeks (p < 0.05). In the tibia at 8 weeks all the samples showed fibrous encapsulation. At 16 weeks fibrous capsules were thinner or occasionally disappeared. Bone ingrowth was noticed in the samples with large glass granules. Further, new bone formation was found in the medullary cavity. No signs of polymer degradation were seen at any time point. It can be concluded that the composite of BAG (S53P4) and copolymer of poly(epsilon-caprolactone-co-DL-lactide) is biocompatible with the bone tissue within the 16 weeks implantation period.

Effect of synthesis parameters of the sol-gel-processed spray-dried silica gel microparticles on the release rate of dexmedetomidine.

The objective of this study was to evaluate the possibilities to control the release rate of dexmedetomidine (DMED) from different spray-dried silica gel microparticle formulations. Microparticles were prepared by spray drying a silica sol polymer solution containing the drug. Drug release was investigated both in vitro and in vivo. The influence of sol-gel synthesis parameters, like pH and the water/alkoxide ratio (r) of the sol, on the release behaviour of the drug was studied. Silica gel microparticles had a smooth surface. Microparticles prepared from diluted sol, however, were more aggregated and clustered. The drug release conformed to zero order release from microparticles prepared near the isoelectric point of silica (pH 2.3 and pH 3) and to the square root of time kinetics from microparticles prepared at pH 1 and pH 5. The release also showed a dual-phasic profile with an initial burst and after that a slower release period. The dexmedetomidine release conformed to zero order kinetics from microparticles prepared at water/ alkoxide ratios between r = 6 and r = 35 (at pH 2.3). The release rate was the slowest from microparticles prepared with water/ alkoxide ratio 35. The bioavailability of dexmedetomidine in dogs showed that the release was sustained from silica gel microparticles as compared with a subcutaneously administered reference dose of 0.1 mg.

In vitro evaluation of poly(epsilon-caprolactone-co-DL-lactide)/ bioactive glass composites.

In vitro bioactivity of composites of poly(epsilon-caprolactone-co-DL-lactide) P(CL/DL-LA) containing different amounts (40, 60 and 70 wt%) of bioactive glass, S53P4, was evaluated. Two ranges of granule size of bioactive glass (< 45 microm and 90-315 microm) were blended with P(CL/DL-LA) copolymer in a batch mixer. The composites were characterised by dynamic mechanical thermal analysis. The molecular weight and the melting temperature of the copolymer matrix were adjusted to enable the application of the composite material by injection below 50 degrees C. Formation of Ca-P deposition on the surface of the composites after dissolution in simulated body fluid at 37 degrees C was recorded by scanning electron microscopy. Degradation of the composite material was measured by water absorption and changes in the average molecular weights as a function of the dissolution time. In vitro bioactivity was found to be dependent on the weight fraction and granule size range of the bioactive glass used. The presence of the bioactive filler also accelerated the degradation compared with the neat polymer sample.