Cyclodextrin and TiF4 Nanocomplex on Enamel Demineralization.

The aim of this study was to assess the effect of a newly developed nanocomplex formed of hydroxypropyl-b-cyclodextrin and 1% titanium tetrafluoride (TiF4) after distinct complexation periods (12/72 h) on demineralization of bovine enamel in vitro. Enamel blocks (n=60) were allocated in different groups: Mili-Q water, hydroxypropyl-b-cyclodextrin, 1% TiF4, hydroxypropyl-b-cyclodextrin + 1% TiF4 after 12 h of complexation and hydroxypropyl-b-cyclodextrin + 1% TiF4 after 72 h of complexation. The samples were evaluated by surface microhardness, cross-sectional microhardness and micro-CT. Scanning electron microscopy and energy dispersive X-ray spectrometry (SEM/EDX) were also obtained. Hydroxypropyl-b-cyclodextrin + 1% TiF4 after 12 h complexation resulted in lower percentage of surface microhardness loss compared to Mili-Q water, hydroxypropyl-b-cyclodextrin, 1% TiF4 and hydroxypropyl-b-cyclodextrin + 1% TiF4 after 72 h of complexation group, with a large effect size (from 1.307 to 2.943) and high power (84.9 to 99%). All groups resulted in similar integrated mineral loss (ΔZ) obtained by both internal microhardness and micro-CT techniques. Enamel treated with TiF4 and TiF4 + hydroxypropyl-b-cyclodextrin groups showed a TiO2 glaze-layer, while EDX evaluation identified Ti. The solution containing the inclusion complex of hydroxypropyl-b-cyclodextrin + TiF4 with 12 h of complexation period demonstrated a significant ability to reduce surface demineralization of sound enamel under an artificial cariogenic challenge.

Cyclodextrin and TIF4 nanocomplex on enamel demineralization

Abstract The aim of this study was to assess the effect of a newly developed nanocomplex formed of hydroxypropyl-b-cyclodextrin and 1% titanium tetrafluoride (TiF4) after distinct complexation periods (12/72 h) on demineralization of bovine enamel in vitro. Enamel blocks (n=60) were allocated in different groups: Mili-Q water, hydroxypropyl-b-cyclodextrin, 1% TiF4, hydroxypropyl-b-cyclodextrin + 1% TiF4 after 12 h of complexation and hydroxypropyl-b-cyclodextrin + 1% TiF4 after 72 h of complexation. The samples were evaluated by surface microhardness, cross-sectional microhardness and micro-CT. Scanning electron microscopy and energy dispersive X-ray spectrometry (SEM/EDX) were also obtained. Hydroxypropyl-b-cyclodextrin + 1% TiF4 after 12 h complexation resulted in lower percentage of surface microhardness loss compared to Mili-Q water, hydroxypropyl-b-cyclodextrin, 1% TiF4 and hydroxypropyl-b-cyclodextrin + 1% TiF4 after 72 h of complexation group, with a large effect size (from 1.307 to 2.943) and high power (84.9 to 99%). All groups resulted in similar integrated mineral loss (ΔZ) obtained by both internal microhardness and micro-CT techniques. Enamel treated with TiF4 and TiF4 + hydroxypropyl-b-cyclodextrin groups showed a TiO2 glaze-layer, while EDX evaluation identified Ti. The solution containing the inclusion complex of hydroxypropyl-b-cyclodextrin + TiF4 with 12 h of complexation period demonstrated a significant ability to reduce surface demineralization of sound enamel under an artificial cariogenic challenge.

Resumo O objetivo deste estudo foi avaliar o efeito da 1-etil-3- (3-dimetilaminopropil) carbodiimida (EDC) na resistência de união de pinos de fibra de vidro em canais radiculares obturados com diferentes cimentos endodônticos. Setenta e oito pré-molares inferiores foram obturados com três cimentos endodônticos (n=26): Endofill (END), AH Plus (AHP) e Endosequence BC Sealer (EBS). Após o preparo do espaço para pino, dois subgrupos formaram-se conforme a cimentação dos pinos (n=13): com EDC e sem EDC (controle - CON). Os espécimes foram submetidos ao teste pull-out, classificação do modo de falha e avaliação da superfície do canal radicular por microscopia eletrônica de varredura após o deslocamento. Quanto à força de resistência de união, uma diferença estatisticamente significativa ocorreu entre os subgrupos EDC e CON apenas no END (p=0,001). Não foi detectada diferença entre os subgrupos CON (p=0,339). Contudo, no subgrupo EDC, o AHP apresentou maiores valores (END versus AHP: p=0,001; AHP versus EBS: p=0,016). Acerca da classificação dos modos de falha, o escore 1 (≥50% de cimento) foi o mais comumente observado, exceto para END + EDC. Restos de cimentos endodônticos e cimentos resinosos foram encontrados no terço cervical, mas sem diferença estatística (p=0,269), enquanto no terço médio, houve diferença (p=0,004). Em conclusão, o EDC diminui a resistência de união quando associado ao cimento END, sem alterar o modo de falha entre o cimento resinoso e o pino de fibra de vidro. O melhor desempenho foi observado quanto o EDC foi usado com o cimento AHP.

Characterization and effect of nanocomplexed fluoride solutions on the inhibition of enamel demineralization created by a multispecies cariogenic biofilm model.

OBJECTIVES: The aim of this study was to assess the in vitro caries preventive effect of nanocomplexed solutions of hydroxypropyl-ß-cyclodextrin and γ-cyclodextrin associated with titanium tetrafluoride (TiF4) after different complexation times (12 or 72 h). MATERIALS AND METHODS: Enamel blocks were randomly distributed in 9 groups (n = 11): negative control, hydroxypropyl-ß-cyclodextrin, γ-cyclodextrin, TiF4, hydroxypropyl-ß-cyclodextrin:TiF4 12 h, hydroxypropyl-ß-cyclodextrin:TiF4 72 h, γ-cyclodextrin:TiF4 12 h, γ-cyclodextrin:TiF4 72 h, and NaF (positive control). The solutions were applied for 1 min and the blocks were exposed to a biofilm model. Nanocompounds were characterized by differential scanning calorimetry and X-ray powder diffraction. The percentage of surface microhardness loss (%SML), mineral density changes (ΔZ), lesion depth, surface morphology (scanning electron microscopy-SEM), and chemical characterization (energy-dispersive spectroscopy-EDS) were assessed. RESULTS: No oxidation was observed, and the formation of the nanocomplexes was evidenced by changes in the melting point compared to pure cyclodextrins and the loss of crystallinity of the materials. Hydroxypropyl-ß-cyclodextrin:TiF4 72 h resulted in lower %SML than negative control, hydroxypropyl-ß-cyclodextrin, γ-cyclodextrin, and TiF4 (p < 0.05). NaF differed from all groups (p < 0.05), except for hydroxypropyl-ß-cyclodextrin:TiF4 72 h (p = 0.83). ΔZ of hydroxypropyl-ß-cyclodextrin:TiF4 72 h was higher than negative control, hydroxypropyl-ß-cyclodextrin, γ-cyclodextrin, γ-cyclodextrin:TiF4 1 2 h, γ-cyclodextrin:TiF4 72 h, and NaF (p < 0.05) and similar to TiF4 and hydroxypropyl-ß-cyclodextrin:TiF4 12 h (p > 0.05). SEM/EDS detected Ti in the blocks subjected to TiF4-products. CONCLUSION: The hydroxypropyl-ß-cyclodextrin:TiF4 72 h solution showed caries preventive effect on the surface and subsurface of the enamel. CLINICAL RELEVANCE: A hydroxypropyl-ß-cyclodextrin nanosystem, in association with TiF4 after 72 h of complexation, may be a promising agent for the prevention of enamel demineralization.

Micro-tensile bond strength and interfacial characterization of an adhesive bonded to dentin prepared by contemporary caries-excavation techniques.

OBJECTIVES: To evaluate the micro-tensile bond strength (µTBS) and interfacial characteristics of adhesive-dentin bonds produced after caries-removal with contemporary techniques. METHODS: Carious molars were cut at the base of the fissure, exposing 'sound' and 'carious' dentin at different spots. After caries-excavation, a composite was bonded using a 2-step self-etch adhesive. The µTBS was measured and the mode of fracture analyzed using a stereomicroscope and imaged by Feg-SEM, while additional non-fractured specimens were histologically analyzed after Masson's trichrome staining in order to identify potentially incompletely resin-enveloped collagen. RESULTS: µTBS to residual caries-excavated dentin was lower than to sound dentin. The different caries-removing techniques had a significant effect on the µTBS. Er:YAG laser guided by a LIF-feedback system (Kavo) resulted in the lowest µTBS (26.8% lower than to 'sound' dentin) and a distinct layer of incompletely resin-enveloped collagen at the interface. Although different degrees of collagen exposure were seen for other caries-removing techniques, such as a thick layer for CeraBur (Komet-Brasseler), some unprotected collagen areas for Cariex (Kavo), or completely resin-enveloped collagen for a tungsten-carbide-bur (Komet), the µTBS appeared not directly affected (10%, 16.6%, and 15.3% lower than to 'sound' dentin, respectively). Carisolv (MediTeam) resulted in the highest µTBS (only 1% reduction compared to that to 'sound' dentin), followed by the tungsten-carbide-bur aided by Caries Detector (Kuraray) (4.8% reduction). Enzymatic caries excavation using the experimental SFC-VIII (3M-ESPE) aided by a disposable plastic instrument resulted in a 19.4% reduction in µTBS as compared to that to 'sound' dentin. SIGNIFICANCE: The dentin bonding receptiveness depends to a large extent on the caries-excavation method employed.

Caries-removal effectiveness and minimal-invasiveness potential of caries-excavation techniques: a micro-CT investigation.

OBJECTIVES: To determine the caries-removal effectiveness (CRE) and minimal-invasiveness potential (MIP) of contemporary caries-removal techniques. METHODS: Carious molars were scanned using micro-CT, after which dentine caries was removed by 9 contemporary caries-removal techniques. The micro-CT was repeated and CRE was determined on basis of the relative volume of residual caries and the mineral density (MD) at the cavity floor. MIP was determined by measuring the cavity size relative to the initial size of the caries lesion. RESULTS: CRE and MIP varied most for the Er:YAG laser (Kavo) despite its laser-induced fluorescence (LIF) feedback system. Whilst some specimens revealed much residual caries, others showed over-excavation into sound dentine. With the highest Relative Cavity Size, the Er:YAG laser presented the lowest MIP. Rotary/oscillating instruments revealed a more favourable CRE with some tendency towards over-excavation, except for CeraBur (Komet-Brasseler) and Cariex (Kavo) that typically left caries at the cavity floor and cavity walls, respectively. Chemo-mechanical excavation aided by conventional metal excavators (Carisolv, MediTeam; exp. SFC-V and SFC-VIII, 3M-ESPE) combined best CRE with MIP. When however a plastic excavator was used along with exp. SFC-VIII, caries was less completely removed. SIGNIFICANCE: Er:YAG-laser aided by LIF resulted in non-selective caries removal. Rotary/oscillating caries removal may lead to over-excavation, especially when burs are combined with Caries Detector (Kuraray). This risk for over-excavation is reduced when a tungsten-carbide bur is solely used. On the contrary, Cariex (Kavo) and CeraBur showed a tendency for under-preparation. Chemo-mechanical methods were most selective in removing caries, whilst preserving sound tissue.

Micro-CT based quantitative evaluation of caries excavation.

OBJECTIVES: To optimize a microtomographic (micro-CT) technique to quantitatively evaluate the effectiveness of contemporary caries-excavation techniques. METHODS: A beam-hardening curve was obtained from an initial reconstruction of a wedge-shaped hydroxyapatite (HAp) block and fitted with a 5th order polynomial function, after which each micro-CT tooth slice was corrected accordingly. Calibration of the 8-bit gray values into mineral-density values was obtained by scanning, reconstructing and processing volume of interests (VOIs) of HAp phantoms with different mineral densities (0.25, 0.75, 3.14g/cm(3)). One carious tooth was scanned before and after caries removal with an experimental enzyme-based gel. After reconstruction, a 3D-median filter was applied to each micro-CT slice, and a connected threshold grower algorithm was used to blank-out undesired structures in each slice. Volume rendering with a look-up-table (LUT), based on mineral densities, was accomplished for the tooth before and after caries removal. Finally, the actual volume of excavated tissue was quantified. RESULTS: Correction for beam hardening produced tooth slices with relatively homogeneous gray values along the whole area of enamel and dentin. Accurate mineral-density values were obtained for enamel, dentin and carious regions (2.89, 1.74 and 0.27g/cm(3), respectively). After pre-processing (3D-median filtering and connected threshold grower algorithm), acceptable segmentation of carious dentin based on gray values was accomplished (Otsu method, gray value=75 or mineral density=1.12g/cm(3)), from which quantitative volumetric parameters were calculated. SIGNIFICANCE: Accurate calibration, standardization of scanning and reconstruction steps and adequate pre-processing of micro-CT slices allowed detailed volumetric calculation of caries-excavation techniques.

Influence of joint component mechanical properties and adhesive layer thickness on stress distribution in micro-tensile bond strength specimens.

OBJECTIVES: Differences in mechanical properties between adherents and adhesive result in stress singularity at the free edge for tensile test specimens. Beyond causing premature failures, these also trigger fracture initiation at the bond edge, where the use of the maximum stress at failure as a measure of strength is not a reliable parameter for obtaining bond strength. The aim of this study is to describe the pattern of stress concentration along the interface for micro-tensile bond strength (microTBS) specimens. Also, possible sources of variation in stress concentration (adhesive layer thickness and mechanical properties) were evaluated using the finite element method. METHODS: One-fourth models of typical microTBS specimens were created using axisymmetric elements. A 15MPa load was applied at the outer edge and finite element calculations were performed within the elastic deformation range. In the first set of runs, the adhesive thickness was varied and in the second set, different nu/E ratios between the adhesive and the adherent were assigned. RESULTS: When adhesive thickness increased, a significant increase in stress concentration at the free edge and in the length of the stress-affected area was observed. Increasing the nu/E ratio between adhesive and adherent lead to an increase in stress concentration at the free edge area without change in length of the stress-affected area. SIGNIFICANCE: If mechanical properties and adhesive thickness expected for a specific composite-dentin bond combination in microTBS specimens are known, stress concentration at the interface can be predicted. The adhesive thickness should remain constant when comparing different joints, as it facilitates the interpretation of nominal strength values.

Influence of notch geometry and interface on stress concentration and distribution in micro-tensile bond strength specimens.

OBJECTIVES: Describe stress distribution and compare stress concentration factor (K(t)) for homogeneous micro-specimens with different notch geometries and stick-shaped homogeneous and bimaterial specimens by means of finite element (FE) analysis. METHODS: Axisymmetric models were created for homogeneous specimens with different notches and for stick-shaped homogeneous and bimaterial specimens. FE mesh was refined at areas of expected stress concentration and boundary conditions included an applied tensile stress in the axial direction. Linear elastic analysis was used. RESULTS: For hourglass homogeneous specimens, K(t) equaled 1.32 and 1.12 for a notch radius of 0.6mm and 3.3mm, respectively. A non-uniform axial (sigma(zz)) stress distribution was found in the notch cross-section, with values at the outer edge being 78% and 25% larger than at the center. In addition, a triaxial stress state was generated. Stick-shaped and dumbbell homogeneous specimens presented K(t)=1 and a uniform, uniaxial stress distribution along the entire cross-section. Shear stresses were zero for all homogeneous specimens. When an adhesive interface was added to the stick-shaped specimen, an area of localized axial stress concentration (K(t)=1.55) was detected at the bimaterial joint near the outer edge. Normal stresses sigma(rr) and sigma(thetatheta) and shear stress tau(zr) were also non-zero at the free-edge. CONCLUSIONS: Dumbbell or stick-shaped specimens are favored for muTBS testing, as they do not present stress concentrations due to geometry. However, dissimilar mechanical properties of joint components will lead to stress concentrations and non-uniform multi-axial stresses, although to a lesser extent.