Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: dissolution behaviour and biological properties after crystallisation.

Hydroxyapatite (HA), fluor-hydroxyapatite (FHA) with varying levels of fluoride ion substitution and fluorapatite (FA) were synthesised by the sol-gel method as possible implant coating or bone-grafting materials. Calcium nitrate and triethyl phosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride were incorporated for the preparation of the FHA and FA sol-gels. After heating and powdering the sol-gels, dissolution behaviour was assessed using ion chromatography to measure Ca(2+) and PO4 (3-) ion release. Biological behaviour was assessed using cellular proliferation with human osteosarcoma cells and alamarBlue™ assay. Statistical analysis was performed with a two way analysis of variance and post hoc testing with a Bonferroni correction. Increasing fluoride substitution into an apatite structure decreased the dissolution rate. Increasing the firing temperature of the HA, FHA and FA sol-gels up to 1,000 °C decreased the dissolution rate. There was significantly higher cellular proliferation on highly substituted FHA and FA than on HA or Titanium. The properties of an implant coating or bone grafting material can be tailored to meet specific requirements by altering the amount of fluoride that is incorporated into the original apatite structure. The dissolution behaviour can further be altered by the temperature at which the sol-gel is fired.

Effect of Different Decontamination Methods on Fracture Resistance, Microstructure, and Surface Roughness of Zirconia Restorations-In Vitro Study.

This study aimed to evaluate the effect of seven different decontamination methods (water, ZirCleanTM, 37% phosphoric acid, 9.5% hydrofluoric acid, Al2O3 sandblasting, low-speed dental stone, and high-speed dental stone) on the fracture resistance, microstructure, and surface roughness of monolithic and multilayered zirconia. The as-received and sandblasted zirconia was used as a control. One-way ANOVA and t-test were performed. As-received monolithic zirconia was stronger (856 ± 94 MPa) than multilayered zirconia (348.4 ± 63 MPa). Only phosphoric acid (865 ± 141 MPa) and low-speed dental stone (959 ± 116 MPa) significantly increased the flexural strength of sandblasted monolithic zirconia (854 ± 99 MPa), but all tested decontamination methods except phosphoric acid (307 ± 57 MPa) and Al2O3 (322 ± 69 MPa) significantly increased the flexural strength of sandblasted multilayered zirconia (325 ± 74 MPa). Different decontamination methods did not significantly affect the flexural modulus, but introduced irregularities in the crystal as well as deep surface flaws in both types of zirconia. The surface of sandblasted monolithic zirconia is more resistant to change than multilayered zirconia. Among different decontamination methods, a low-speed dental stone could be beneficial as it significantly increased the surface roughness and fracture resistance of both types of zirconia.

Cyclic shear fatigue of orthodontic brackets bonded to enamel using self-adhering flowable composites.

Background: Self-adhering composites are claimed to bond to teeth without prior acid etching and bonding steps. This study aimed to evaluate the cyclic shear fatigue (CSF) of metal orthodontic brackets bonded to enamel using self-adhering flowable composites (Constic and VertiseTM Flow) in comparison with that of total-etch and self-etch adhesives. Materials and methods: Twenty-five human premolars comprising 100 surfaces were randomly divided into four groups (n = 25): total-etch, self-etch, Constic, and VertiseTM Flow. A total of 10 surfaces were used per group for baseline static shear bond strength (SSBS) evaluation and 15 surfaces for CSF evaluation. Each tooth was treated with the four bonding agents. Both SSBS and CSF were evaluated using a universal testing machine. For CSF, the staircase method was used with an initial pulling load equivalent to 60% of the SSBS of each group for 1000 cycles or until failure. The adhesive remaining index (ARI) was evaluated for surviving samples using a stereomicroscope. Statistical analysis: A one-way ANOVA with Tukey's post hoc test was used to analyze the CSF data, and a chi-square test was used to analyze the ARI. Results: The total-etch adhesive showed significantly higher CSF values than that of the other groups (p < 0.001). Both total-etch (10.78 ± 0.31 MPa) and self-etch (6.75 ± 0.91 MPa) adhesives showed significantly higher CSF than did Constic (1.94 ± 0.31 MPa) and VertiseTM Flow (2.01 ± 0.25 MPa), (p < 0.001). The ARI indicated that more resin remnants were observed with the total-etch and self-etch adhesives than those with the self-adhering flowable composites. However, no significant differences were observed among groups (p > 0.05). Conclusions: Total-etch and self-etch adhesives showed satisfactory bond strengths for orthodontic treatment. However, Constic and VertiseTM Flow self-adhering flowable composites may not be clinically sufficient for bonding metallic orthodontic brackets to enamel.

Biocompatibility and Antibacterial Action of Salvadora persica Extract as Intracanal Medication (In Vitro and Ex Vivo Experiment).

This study aimed to test the biocompatibility and antibacterial properties of Salvadora persica (S. persica) extract, a natural product, as an intracanal medication in comparison with calcium hydroxide (Metapaste, META BIOMED, Cheongju, Korea). The pH values of both materials were tested. The biocompatibility of S. persica extract and Metapaste was determined using light microscopy and MTT assays. The antibacterial action was tested using the zone of bacterial inhibition on four common bacterial species. In addition, intracanal medication was administered using 68 extracted single-rooted teeth contaminated with Enterococcus faecalis (E. faecalis), and the percentage reduction in colony count (% RCC) at 1, 3, and 7 days was measured. The extension of activity for both materials was assessed using histological sections and scanning electron microscopy. S. persica was found to be acidic in nature. Both materials showed significantly lower cell viability than the positive control cells on days 1 and 3 but not on day 7. S. persica showed better antibacterial effects against E. faecalis and S. mutans. S. persica extract showed 97.6%, 98.9%, and 99.3% RCC values at 1, 3, and 7 days, respectively, which are comparable to those of Metapaste. S. persica herbal extract is a promising material that can be utilized as an intracanal medication, but its use requires further research.

Antibacterial, remineralising and matrix metalloproteinase inhibiting scandium-doped phosphate glasses for treatment of dental caries.

OBJECTIVES: Antibiotic resistance is increasingly a growing global threat. This study aimed to investigate the potential use of newly developed scandium-doped phosphate-based glasses (Sc-PBGs) as an antibacterial and anticariogenic agent through controlled release of Sc3+ ions. METHODS: Sc-PBGs with various calcium and sodium oxide contents were produced and characterised using thermal and spectroscopic analysis. Degradation behaviour, ion release, antibacterial action against Streptococcus mutans, anti-matrix metalloproteinase-2 (MMP-2) activity, remineralisation potential and in vivo biocompatibility were also investigated. RESULTS: The developed glass system showed linear Sc3+ ions release over time. The released Sc3+ shows statistically significant inhibition of S. mutans biofilm (1.2 log10 CFU reduction at 6 h) and matrix metalloproteinase-2 (MMP-2) activity, compared with Sc-free glass and positive control. When Sc-PBGs were mounted alongside enamel sections, subjected to acidic challenges, alternating hyper- and hypomineralisation layers consistent with periods of re- and demineralisation were observed demonstrating their potential remineralising action. Furthermore, Sc-PBGs produced a non-toxic response when implanted subcutaneously for 2 weeks in Sprague Dawley rats. SIGNIFICANCE: Since Sc3+ ions might act on various enzymes essential to the biological mechanisms underlying caries, Sc-PBGs could be a promising therapeutic agent against cariogenic bacteria.

An Eggshell-Based Toothpaste as a Cost-Effective Treatment of Dentin Hypersensitivity.

OBJECTIVES: This study aimed to test the efficacy of two experimentally produced eggshell-based toothpastes on dentinal tubules occlusion. MATERIALS AND METHODS: Two experimental eggshell toothpastes, based on natural ingredients, with or without titanium dioxide nanoparticles (TNPs) were produced and coded "TNPs eggshell toothpaste [TNPsESTP]" or "eggshell toothpaste [ESTP]," respectively. Mid-coronal dentin discs, from 28 human extracted molar teeth, etched with 37% phosphoric acid for 60 seconds to simulate the hypersensitive dentin, were randomly divided into four groups-G1: no treatment (negative control), G2: ESTP treated, G3: TNPsESTP treated, and G4: Biorepair treated (positive control). All treated discs were brushed for 2 weeks and 1 month using a toothbrush simulator at 40 mm/s. Dentinal tubules occlusion was studied using a cross-polarization optical coherence tomography (CP-OCT) and scanning electron microscopy (SEM). STATISTICAL ANALYSIS: Unpaired t-test was conducted using GraphPad software (San Diego, California, United States). Continuous variables were expressed as means ± standard deviation and p < 0.05 was considered statistically significant. RESULTS: From CP-OCT, a marked increase in surface reflectivity of dentin was observed after brushing with tested toothpastes. ESTP and NPsESTP showed higher or comparable grayscale values than Biorepair indicating increase in surface density of dentin. From SEM, at 2 weeks, ESTP showed comparable number of completely occluded dentinal tubules to Biorepair. TNPsESTP showed significantly lower numbers of CODT than Biorepair. At 1 month, the number of CODT was difficult to count for all treated groups. Both ESTP and TNPsESTP showed significantly higher numbers of partially occluded dentinal tubules than Biorepair. CONCLUSION: ESTP or TNPsESTP could offer a cost-effective substitute for the treatment of dentin hypersensitivity.

Structure and properties of strontium-doped phosphate-based glasses.

Owing to similarity in both ionic size and polarity, strontium (Sr2+) is known to behave in a comparable way to calcium (Ca2+), and its role in bone metabolism has been well documented as both anti-resorptive and bone forming. In this study, novel quaternary strontium-doped phosphate-based glasses, containing 1, 3 and 5 mol% SrO, were synthesized and characterized. (31)P magic angle spinning (MAS) nuclear magnetic resonance results showed that, as the Sr2+ content is increased in the glasses, there is a slight increase in disproportionation of Q2 phosphorus environments into Q(1) and Q3 environments. Moreover, shortening and strengthening of the phosphorus to bridging oxygen distance occurred as obtained from FTIR. The general broadening of the spectral features with Sr2+ content is most probably due to the increased variation of the phosphate-cation bonding interactions caused by the introduction of the third cation. This increased disorder may be the cause of the increased degradation of the Sr-containing glasses relative to the Sr-free glass. As confirmed from elemental analysis, all Sr-containing glasses showed higher Na2O than expected and this also could be accounted for by the higher degradation of these glasses compared with Sr-free glasses. Measurements of surface free energy (SFE) showed that incorporation of strontium had no effect on SFE, and samples had relatively higher fractional polarity, which is not expected to promote high cell activity. From viability studies, however, the incorporation of Sr2+ showed better cellular response than Sr(2+)-free glasses, but still lower than the positive control. This unfavourable cellular response could be due to the high degradation nature of these glasses and not due to the presence of Sr2+.

Morphological and Spectroscopic Study of an Apatite Layer Induced by Fast-Set Versus Regular-Set EndoSequence Root Repair Materials.

This study aimed to evaluate the morphology and chemistry of an apatite layer induced by fast-set versus regular-set EndoSequence root repair materials using spectroscopic analysis. Holes of a 4 mm diameter were created in the root canal dentin, which were filled with the test material. Fetal calf serum was used as the incubation medium, and the samples incubated in deionized water were used as controls. The material-surface and material-dentin interfaces were analyzed after 28 days using Raman and infrared spectroscopy, scanning electron microscopy/energy dispersive X-ray, and X-ray diffraction. After incubation in fetal calf serum, both materials formed a uniform layer of calcium phosphate precipitate on their surfaces, with the dentinal interface. This precipitated layer was a combination of hydroxyapatite and calcite or aragonite, and had a high mineral maturity with the regular-set paste. However, its crystallinity index was high with the fast-set putty. Typically, both consistencies (putty and paste) of root repair material have an apatite formation ability when they are incubated in fetal calf serum. This property could be beneficial in improving their sealing ability for root canal dentin.

Sodium Hypochlorite Irrigation and Its Effect on Bond Strength to Dentin.

Effective shaping and cleaning of root canals are essential for the success of endodontic treatment. Due to the complex anatomy of root canal spaces, the use of various instrumentation techniques alone is not effective in producing bacteria-free root canal spaces. Irrigation, disinfectants, rinses, and intervisit medications are used in conjunction with the mechanical instrumentation to ensure the success of endodontic treatment. Sodium hypochlorite (NaOCl), a halogenated compound, is routinely used to irrigate the root canal during endodontic treatments. NaOCl has been known for its antibacterial action, proteolytic and dissolution capacity, and debridement properties. NaOCl, however, can alter the composition of dentin and hence its interaction with the adhesive resins used to bond the restorative materials to treated dentin. This review therefore covers in depth the action of NaOCl on dentin-adhesive resin bond strength including both enhancement and reduction, then mechanisms proposed for such action, and finally how the adverse action of NaOCl on dentin can be reversed.

Surface characterisation of various bone cements prepared with functionalised methacrylates/bioactive ceramics in relation to HOB behaviour.

This study reports the relationship between the biocompatibility and surface properties of experimental bone cements. The effect of hydroxyapatite (HA) or alpha-tri-calcium phosphate (alpha-TCP) incorporated into bone cements prepared with methyl methacrylate as base monomer and either methacrylic acid or diethyl amino ethyl methacrylate (DEAEMA) as comonomers was investigated. The in vitro biocompatibility of these composite cements was assessed in terms of the interaction of primary human osteoblasts grown on the materials over a period of 5 days and compared with a control surface. These results were related to the surface properties investigated through a number of techniques, namely Fourier transform infrared, contact angle measurements, X-ray photoelectron spectroscopy and energy dispersive analysis of X-rays. Complementary techniques of thermal analysis and ion chromatography were also performed. Biocompatibility results showed that the addition of alpha-TCP improves biocompatibility regardless of comonomer type. This is in contrast to HA-based cements where cell proliferation was significantly lower. Surface characterisations showed that structural integrity of the materials was maintained in the presence of the acid and base comonomers, and water contact angles were reduced particularly in DEAEMA containing materials. Furthermore, ion chromatography confirmed higher Ca2+ and PO4(3-) ion release by both types of ceramics, particularly for those containing DEAEMA. In conclusion, the incorporation of acidic and basic comonomers to either HA or alpha-TCP ceramics containing bone cements can have differential effects upon the attachment and proliferation of bone cells in vitro. Moreover, those cements consisting of alpha-TCP and containing DEAEMA comonomer indicated the most favourable biocompatibility.

Development of dental composites with reactive fillers that promote precipitation of antibacterial-hydroxyapatite layers.

The study aim was to develop light-curable, high strength dental composites that would release calcium phosphate and chlorhexidine (CHX) but additionally promote surface hydroxyapatite/CHX co-precipitation in simulated body fluid (SBF). 80 wt.% urethane dimethacrylate based liquid was mixed with glass fillers containing 10 wt.% CHX and 0, 10, 20 or 40 wt.% reactive mono- and tricalcium phosphate (CaP). Surface hydroxyapatite layer thickness/coverage from SEM images, Ca/Si ratio from EDX and hydroxyapatite Raman peak intensities were all proportional to both time in SBF and CaP wt.% in the filler. Hydroxyapatite was, however, difficult to detect by XRD until 4 weeks. XRD peak width and SEM images suggested this was due to the very small size (~10 nm) of the hydroxyapatite crystallites. Precipitate mass at 12 weeks was 22 wt.% of the sample CaP total mass irrespective of CaP wt.% and up to 7 wt.% of the specimen. Early diffusion controlled CHX release, assessed by UV spectrometry, was proportional to CaP and twice as fast in water compared with SBF. After 1 week, CHX continued to diffuse into water but in SBF, became entrapped within the precipitating hydroxyapatite layer. At 12 weeks CHX formed 5 to 15% of the HA layer with 10 to 40 wt.% CaP respectively. Despite linear decline of strength and modulus in 4 weeks from 160 to 101 MPa and 4 to 2.4 GPa, respectively, upon raising CaP content, all values were still within the range expected for commercial composites. The high strength, hydroxyapatite precipitation and surface antibacterial accumulation should reduce tooth restoration failure due to fracture, aid demineralised dentine repair and prevent subsurface carious disease respectively.

Root maturation and dentin-pulp response to enamel matrix derivative in pulpotomized permanent teeth.

The success of pulpotomy of young permanent teeth depends on the proper selection of dressing materials. This study aimed to evaluate the histological and histomorphometric response of dentin-pulp complex to the enamel matrix derivative (Emdogain(®) gel) compared to that of calcium hydroxide when used as a pulp dressing in immature young permanent dogs' teeth. Dentin-like tissues bridging the full width of the coronal pulp at the interface between the injured and healthy pulp tissues were seen after 1 month in both groups. With time, the dentin bridge increased in thickness for calcium hydroxide but disintegrated and fully disappeared for Emdogain-treated group. Progressive inflammation and total pulp degeneration were only evident with Emdogain-treated group. The root apices of Emdogain-treated teeth became matured and closed by cementum that attached to new alveolar bone by a well-oriented periodontal ligament. In young permanent dentition, Emdogain could be a good candidate for periodontium but not dentino-pulpal complex regeneration.

Collagen--emerging collagen based therapies hit the patient.

The choice of biomaterials available for regenerative medicine continues to grow rapidly, with new materials often claiming advantages over the short-comings of those already in existence. Going back to nature, collagen is one of the most abundant proteins in mammals and its role is essential to our way of life. It can therefore be obtained from many sources including porcine, bovine, equine or human and offer a great promise as a biomimetic scaffold for regenerative medicine. Using naturally derived collagen, extracellular matrices (ECMs), as surgical materials have become established practice for a number of years. For clinical use the goal has been to preserve as much of the composition and structure of the ECM as possible without adverse effects to the recipient. This review will therefore cover in-depth both naturally and synthetically produced collagen matrices. Furthermore the production of more sophisticated three dimensional collagen scaffolds that provide cues at nano-, micro- and meso-scale for molecules, cells, proteins and bulk fluids by inducing fibrils alignments, embossing and layered configuration through the application of plastic compression technology will be discussed in details. This review will also shed light on both naturally and synthetically derived collagen products that have been available in the market for several purposes including neural repair, as cosmetic for the treatment of dermatologic defects, haemostatic agents, mucosal wound dressing and guided bone regeneration membrane. There are other several potential applications of collagen still under investigations and they are also covered in this review.

Viscoelastic and biological performance of low-modulus, reactive calcium phosphate-filled, degradable, polymeric bone adhesives.

The aim of this study was to investigate the effect of reactive mono- and tricalcium phosphate addition on the mechanical, surface free energy, degradation and cell compatibility properties of poly(lactide-co-propylene glycol-co-lactide) dimethacrylate (PPGLDMA) thin films. Dry composites containing up to 70 wt.% filler were in a flexible rubber state at body temperature. Filler addition increased the initial strength and Young's modulus and reduced the elastic and permanent deformation under load. The polymer had high polar surface free energy, which might enable greater spread upon bone. This was significantly reduced by filler addition but not by water immersion for 7 days. The samples exhibited reduced water sorption and associated bulk degradation when compared with previous work with thicker samples. Their cell compatibility was also improved. Filler raised water sorption and degradation but improved cell proliferation. The materials are promising bone adhesive candidates for low-load-bearing areas.

Titanium and strontium-doped phosphate glasses as vehicles for strontium ion delivery to cells.

This study investigated the use of a Ti-containing quaternary phosphate glass system P(2)O(5)-Na(2)O-CaO-TiO(2) as a vehicle for strontium ion delivery to cells. Four glass compositions were manufactured: 0.5P(2)O(5)-0.15Na(2)O-0.05TiO(2)-(0.3 - x)CaO-xSrO (x = 0, 0.01, 0.03, and 0.05). Structural characterization revealed that sodium calcium phosphate is the dominant phase in all the glasses. Degradation studies demonstrated highly linear glass degradation, with Sr-containing glasses degrading at higher rates than the Sr-free glass. Biocompatibility studies using MG63 cells showed that the Sr-containing glasses possess excellent cell attachment and growth, particularly over short periods (~4 days).

Chemical characterization of a degradable polymeric bone adhesive containing hydrolysable fillers and interpretation of anomalous mechanical properties.

An experimental, light-curable, degradable polyester-based bone adhesive reinforced with phosphate glass particles ((P(2)O(5))(0.45)(CaO)(x)(Na(2)O)(0.55-)(x), x=0.3 or 0.4mol) or calcium phosphate (monocalcium phosphate/beta-tricalcium phosphate (MCPM/beta-TCP)) has been characterized. Early water sorption (8wt.% at 1week) by the unfilled set adhesive catalysed subsequent bulk degradation (4wt.% at 2weeks) and substantial decline in both elastic and storage moduli. Addition of phosphate glass fillers substantially enhanced this water sorption, catalysed greater bulk mass loss (40-50 and 52-55wt.%, respectively) but enabled generation of a microporous scaffold within 2weeks. The high levels of acidic polymer degradation products (38-50wt.% of original polymer) were advantageously buffered by the filler, which initially released primarily sodium trimetaphosphate (P(3)O93-). Calcium phosphate addition raised polymer water sorption to a lesser extent (16wt.%) and promoted intermediate early bulk mass loss (12wt.%) but simultaneous anomalous increase in modulus. This was attributed to MCPM reacting with absorbed water and beta-TCP to form more homogeneously dispersed brushite (CaHPO(4)) throughout the polymer. Between 2 and 10weeks, linear erosion of both polymer (0.5wt.%week(-1)) and composites (0.7-1.2wt.%week(-1)) occurred, with all fillers providing long-term buffer action through calcium and orthophosphate (PO43-) release. In conclusion, both fillers can raise degradation of bone adhesives whilst simultaneously providing the buffering action and ions required for new bone formation. Through control of water sorption catalysed filler reactions, porous structures for cell support or substantially stiffer materials may be generated.