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Elution parameters and HPLC-detection of single components from resin composite.

The toxic effects of mercury derived from amalgam fillings have been a focus of controversy in Germany during the last 25 years. As alternatives to amalgam, composites are used widely to restore anterior and posterior permanent teeth. This study quantifies the amount of TEGDMA and methacrylic acid that can be derived from a polymerized commercial hybrid composite material. Different specimens were made with different curing methods with and without an oxygen inhibition layer. To simulate the removal of composite fillings, some samples were pulverized. The specimens were eluted in distilled water at 37 degrees C for different time intervals. To check the influence of acid conditions, pulverized material was incubated in 6 M HCl. The separation of the eluted chemical resin components was done by HPLC. A defined mixture of pure components was used as an external standard for the identification and quantification of the eluted components. The results focus on the release of triethylengly-coldimethacrylate (TEGDMA) and methacrylic acid. Concerning the different incubation methods, the results showed higher TEGDMA elution with oxygen inhibited surface layer and with the pulverized samples. Within acid conditions, the amount of TEGDMA found was low, but the amount of methacrylic acid increased. Small resin monomers like TEGDMA are primarily eluted from composite in aqueous solutions. Within acid conditions a hydrolytic disintegration of the ester bonding of the monomers could be observed. Methacrylic acid--a substance with allergenic potential--could be detected.

Bisphenol A-Glycidyl Methacrylate↗

In vitro dentine permeability: the relative effect of a dentine bonding agent on crown preparations.

OBJECTIVE: The aim of this study was to determine whether a dentine bonding agent (DBA) had an effect in reducing fluid filtration under cemented provisional crowns. METHODS: Crown preparations on 34 premolars, randomly allocated to two equal-sized test and control groups, were assessed for dentine permeability by a fluid filtration technique. In the test group, prepared crowns were acid-etched and then treated with a DBA (Prime & Bond NT). In the control group, no such DBA was applied. Provisional crowns were cemented on both groups of teeth using non-eugenol zinc oxide cement. Fluid filtration rates were measured repeatedly after crown preparation, at cementation, 1 h, 1 day, 1 week and 3 weeks following crown cementation for both groups. Filtration rates were also measured after acid-etching and dentine bonding for the test group. RESULTS: There was insufficient evidence to suggest any statistically significant differences either between the two groups or, on average, across the five time points in each group in terms of the relative percentage of fluid filtration. CONCLUSION: The DBA used did not seal dentinal tubules any more than did the smear layer and provisional crowns luted with a non-eugenol ZnO cement.

Acid Etching, Dental↗

Mechanical properties of visible light-cured resins reinforced with hydroxyapatite for dental restoration.

OBJECTIVES: The purpose of this study was to measure and analyze the mechanical properties of several composite materials designed for dental restoration. METHODS: The materials were composed of a visible light-curing monomer mixture (either Bis-GMA+TEGDMA or Bis-GMA+HEMA) as a matrix and hydroxyapatite (either microscopic or nanoscopic particles) as a reinforcing filler. The surface of the hydroxyapatite particles was modified by using a coupling agent (citric, malic, acrylic or methacrylic acid). Five specimens of 14 different composites were prepared for each mechanical test: flexural strength, Young's modulus and Vickers hardness. Mean values and standard deviations were calculated, and ANOVA and Student Newman Keuls multiple comparison tests were applied (P < 0.05). RESULTS: The addition of 50-60 wt% of hydroxyapatite particles to the unfilled monomer mixtures led to the increase of both Young's modulus and surface hardness of the material, while the flexural strength decreased. In general, when microscopic instead of nanoscopic hydroxyapatite was used as a reinforcing filler, mechanical properties were favored. The mechanical properties were also improved by adding citric, acrylic or methacrylic acid as a coupling agent. CONCLUSIONS: An adequate surface modification of the hydroxyapatite particles conferred enhanced mechanical properties to the final dental composite. Microscopic-hydroxyapatite particles are preferred to nanoscopic ones.

Acrylates↗

Equilibrium swelling of poly(methacrylic acid-g-ethylene glycol) hydrogels. Effect of swelling medium and synthesis conditions.

Responsive hydrogel networks comprising of poly(methacrylic acid) (PMAA) backbone and oligomeric ethylene glycol (PEG) grafts were synthesized by free-radical solution polymerization and their equilibrium swelling properties were characterized in aqueous solutions of a homologous series of alcohols. These hydrogels are known to exhibit swelling transitions in response to external stimuli which lead to formation or disruption of hydrogen-bonded complexes between the backbone and the grafts. Swelling studies performed in aqueous mixtures of methanol, ethanol and propanol revealed that the effectiveness of an alcohol in breaking the PMAA/PEG complexes increased as the aliphatic segment length of the alcohol was increased. These results confirm the importance of hydrophobic interactions for stabilizing the complexes. Studies performed to determine the effect of the synthesis conditions on the equilibrium swelling properties revealed that the equilibrium degree of swelling increased as the solvent fraction during synthesis was increased. Finally, molecular stimulations revealed that it is sterically possible to form complexes with a 1:1 stoichiometry between chains of poly(methacrylic acid) and poly(ethylene glycol) with essentially no additional bond strain.

Alcohols↗

Targetable HPMA copolymer-adriamycin conjugates. Recognition, internalization, and subcellular fate.

Recognition, internalization, and subcellular trafficking of N-(2-hydroxypropyl)methacrylamide (HPMA) copolymer conjugates containing N-acylated galactosamine (GalN) or monoclonal OV-TL16 antibodies (Ab) have been investigated in human hepatocarcinoma HepG2 and ovarian carcinoma OVCAR-3 cells, respectively. The intrinsic fluorescence of fluorescein or adriamycin (ADR) attached to HPMA copolymers permitted us to follow the subcellular fate of HPMA copolymer conjugates by confocal fluorescence microscopy and fluorescence spectroscopy. The pattern of fluorescence during incubation of HPMA copolymer-ADR-GalN conjugate containing lysosomally degradable tetrapeptide (GFLG) side-chains with HepG2 cells was consistent with conjugate recognition, internalization, localization in lysosomes, followed by the release of ADR from the polymer chains and ultimately diffusion via the cytoplasm into the cell nuclei. A similar pattern was observed in OVCAR-3 cells for Ab targeted HPMA copolymer conjugates. To test our hypothesis that HPMA-copolymer-bound anticancer drugs will be inaccessible to the energy-driven P-glycoprotein efflux pump in multidrug resistant (MDR) cells, we have compared the internalization of the HPMA copolymer-ADR conjugates by sensitive (A2780) and ADR-resistant (A2780/AD) ovarian carcinoma cell lines. Preliminary data on relative retention of ADR in MDR (A2780/AD) cells indicate a higher intracellular ADR concentration after incubation with HPMA copolymer-ADR conjugate when compared to incubation with free (unbound) ADR.

ATP Binding Cassette Transporter, Subfamily B, Mem↗

Surface treatment studies aimed at streamlining fissure sealant application.

Three laboratory studies were carried out with the aim of improving or streamlining enamel surface treatment procedures in fissure sealing. In Study 1, the effect of reducing acid etch time from 60 s to 10 s was assessed by SEM and tensile bond strength measurements. Reduction in etch time produced a finer etch pattern, gave a reduced but still high, bond-strength, albeit with slightly poorer long-term adhesion. Study 2 showed that a conventional acid etch treatment could completely remove acquired pellicle, without prior prophylaxis. SEM studies and bond-strength measurements corroborated this view. In Study 3, compressed air and chemical drying agents were compared for drying speed and efficiency. Compressed air gave more rapid, thorough drying, and greater resultant bond strengths.

Acid Etching, Dental↗

Dyract compomer: comparison of total etch vs. no etch technique.

Different dental materials and methods can influence the integrity of the marginal seal of restorations. To evaluate the microleakage of Dyract AP Light Cured Compomer, a polyacid modified resin (Caulk), using etched and unetched techniques, standardized trapezoidal Class V restorations were placed on facial or lingual surfaces of 20 human molars with the gingival margin in the cementum. Each restoration was scored at the cervical by two independent, double blinded operators, with reference to the DEJ, for dye penetration on a ranking system of: 0 = no evidence of dye penetration; 1 = dye penetration up to one-half the distance to the axial wall; 2 = dye penetration beyond one-half the distance to the axial wall but short of the axial wall; 3 = dye penetration to the axial wall or beyond. Statistical analysis (Fisher Exact Test) indicated that the etched compomer demonstrated significantly less microleakage when compared to the unetched compomer (p < 0.05).

Acid Etching, Dental↗

Microleakage of two new combined primer/adhesive resin systems.

In vitro microleakage of two new combined primer/adhesive systems utilizing the all etch technique (enamel and dentin etch) with the hybrid composite resin TPH is reported. These new combined primer/adhesive systems were compared to the Optibond FL system, which consists of a separate primer and adhesive. Forty Class V preparations were cut on the facial surfaces at the cemento-enamel junction of bovine incisor teeth to a dimension of 2.0 mm x 3.0 mm x 2.0 mm with a 1.0 mm 45 degree incisal bevel. The enamel (incisal) and dentin (gingival) margins were scored separately. Results suggest that Prime & Bond provided an improvement in the gingival marginal seal over the other materials. There was no statistically significant difference in the sealing ability of the materials tested at the incisal margin.

Acid Etching, Dental↗

Effect of caries disclosing agents on bond strengths of total-etch and self-etching primer dentin bonding systems to resin composite.

This study examined the effect of caries disclosing dyes on composite to dentin shear bond strengths of a total etch, one-bottle and two self-etching, non-rinsing primer dental adhesives. Two caries disclosing dyes were evaluated, Seek and Snoop, with three dentin adhesives, Prime & Bond NT, Prompt L-Pop and Clearfil SE Bond. Extracted human molars stored in 0.2% sodium azide were sectioned longitudinally to expose dentin and embedded in acrylic, leaving the dentin exposed. Each dentin adhesive had three test groups (n=12); a control and one with each of the caries disclosing dyes. The control group had the dentin conditioned and the adhesive applied following the manufacturer's instructions. The caries disclosing dye groups had the dentin first treated for 10 seconds with the disclosing dye, rinsed, then the dentin adhesives were applied as in the controls. A column of Tetric Ceram was bonded after dentin adhesive placement to each specimen and light cured. Specimens were stored in room temperature water for 24 hours, thermocycled for 1,000 cycles between 5 degrees C and 55 degrees C and tested in shear until failure. Mean +/- SD shear bond values (SBV) were determined in MPa. A one-way ANOVA and Student Neuman Keuls multiple comparison test within each DBS were performed at a significance level ofp<0.05 to analyze the caries disclosing dyes input on SBV versus the controls. Surface analysis to determine the nature of the type of dentin/composite fracture/ separation was also performed. For the fracture analysis data, a Chi-Square test was performed at a significance level of p<0.05. The results of this study indicate that using the two tested caries disclosing dyes, with a total etch, one bottle and two self-etching, non-rinsing primer dental adhesives did not negatively affect the dentin-to-composite shear bond strengths of the three tested dentin bonding systems (p>0.05).

Acid Etching, Dental↗

The effect of collagen removal and the use of a low-viscosity resin liner on marginal adaptation of resin composite restorations with margins in dentin.

This study evaluated the influence of collagen removal and the use of a low-viscosity liner on the marginal quality of composite restorations for the total-etch system, Prime & Bond 2.1 (PB) and the self-etching primer system, Clearfil SE Bond (CSEB), in high C-factor cavities with margins in dentin. High C-factor cavities were made on dentin exposed from ground labial surfaces of 100 bovine lower incisors, randomly assigned to 10 treatment groups and restored with composite Z 250, placed in bulk. In Group 1 (PB), control group, PB was applied according to the manufacturer's directions; in Group 2 (PB/PLF), an intermediate layer of low-viscosity composite Protect Liner F (PLF) was applied on the bonding resin surface; in Group 3 (PB/SH) following acid-etching, the surfaces were treated with 10% sodium hypochlorite (SH) for one minute and in Group 4 (PB/SH/PLF), the same procedure was conducted as for Group 3, plus an intermediate layer of PLF was applied as for Group 2. In Group 5 (CSEB), the control group, CSEB was applied according to the manufacturer's directions; in Group 6 (CSEB/PLF), an intermediate layer of PLF was applied; in Group 7 (SH/CSEB), the cavity surface was pre-treated with SH; in Group 8 (SH/CSEB/PLF), SH pre-treatment was conducted as for Group 7, then an intermediate layer of PLF was applied; in Group 9 (CSEB/SH), after CSEB-primer application, the surface was treated with SH, followed by CSEB-adhesive application and in Group 10 (CSEB/SH/PLF), the same was conducted as for Group 9, then an intermediate layer of PLF was applied. The specimens were stored at 37 degrees C for 24 hours, polished, molded and replicas were obtained in epoxy resin. The replicas were gold-sputter coated and observed by SEM (300x) for marginal quality classification. The Kruskal-Wallis non-parametrical multi-comparison Test (p<0.05) was used to obtain statistical analysis of the data. Results demonstrated that both adhesive systems in the control groups presented low marginal quality and a high variability. The use of an intermediate layer of PLF significantly improved the marginal quality with the CSEB system but had no effect with the PB system. Collagen depletion with SH enhanced marginal quality for the PB system and did not influence the CSEB system results.

Acetone↗

Morphological characterization of hypersensitive human radicular dentin and the effect of a light-curing resin liner on tubular occlusion.

A dentin biopsy technique was employed to compare the morphological features of hypersensitive and non-sensitive human radicular dentin. Specimens sampled from different areas in the same root surface displaying hypersensitivity or non-sensitivity were prepared for examination in the scanning electron microscope (SEM). Before analysis some specimens were exposed to surface demineralization and digestion of collagen to allow observation of subsurface portions of the dentinal tubules. In another set of observations the potential of a light-curing resin liner to penetrate root dentin in vitro and to maintain tubular occlusion over time following treatment of hypersensitive radicular dentin were examined. Orifices of many dentinal tubules were open in hypersensitive regions while non-sensitive areas generally displayed tubules occluded with mineralized material. SEM-images of HCl-collagenase treated specimens demonstrated the frequent presence of membrane-like structures in tubules of hypersensitive dentin. In non-sensitive dentin these structures were sparse. Topical application of a light-curing resin liner to wedge shaped defects prepared in radicular dentin of extracted human teeth resulted in a surface coating with a resin thickness of 20-50 microns. Resin penetrated dentinal tubules to a depth of more than 5 microns. Dentin biopsies examined 6 months after treatment with the liner showed presence of resin-like material in a majority of the tubules in dentin where hypersensitivity was no longer perceived. In none of the specimens did the liner remain as a surface coating. In areas of recurrent hypersensitivity more than half of the tubules presented with open orifices.(ABSTRACT TRUNCATED AT 250 WORDS)

Acid Etching, Dental↗

Transformations of poly(methoxy hexa(ethylene glycol) methacrylate)-b-(2-(diethylamino)ethyl methacrylate) block copolymer micelles upon metalation.

Micelle transformations upon metalation (i.e., incorporation of metal compounds and metal nanoparticle formation) in poly(methoxy hexa(ethylene glycol) methacrylate)-block-poly((2-(diethylamino)ethyl methacrylate)), PHEGMA-b-PDEAEMA, solutions have been studied using transmission electron microscopy (TEM) and photon correlation spectroscopy (PCS). Three different methods for the formation of metalated micelles are compared: (A) dissolution of the block copolymers in pure water followed by incorporation of platinic acid (H(2)PtCl(6).6H(2)O), (B) micellization in acidic molecular solutions of block copolymers induced by interaction of the protonated amino groups with the PtCl(6)(2)(-) ions, and (C) incorporation of metal species in pH-induced micelles. The latter method leads to well-defined metalated micelles of 22-25 nm diameter containing nanoparticles with diameters of 1.3-1.5 nm. No nanoparticle aggregation is observed. Good agreement is obtained for the sizes of the platinic acid-containing micelles assessed by TEM and PCS.

Light↗

Saucer-shaped cavity preparation for composite resin restorations in class II carious lesions: three-year results.

This study determined the feasibility of saucer-shaped cavity preparations for composite resins in class II lesions. Saucer-shaped class II cavity preparations were restored with composite resin and subjected to clinical, radiographic, and replica cast evaluation (39 restorations) after 6, 18, and 36 months. The results indicated that the retention, resistance form, and wear resistance of the class II saucer-shaped cavity preparations were satisfactory after 3 years.

Acid Etching, Dental↗

Apoptosis induced by the monomers HEMA and TEGDMA involves formation of ROS and differential activation of the MAP-kinases p38, JNK and ERK.

OBJECTIVES: Cytotoxic methacrylate monomers have been identified in aqueous extracts of freshly cured compomers. Some of these compounds, including HEMA and TEGDMA, induce apoptosis and necrosis in vitro. The aim of the present study was to elucidate possible signaling pathways involved in apoptosis following exposure to HEMA or TEGDMA in a salivary gland cell line. METHODS: The cells were exposed to various concentrations of HEMA or TEGDMA. ROS formation was determined by dichlorofluorescein assay. Phosphorylated MAP-kinases ERK1/2, p38 and JNK, as well as specific caspases were identified by Western blotting. Apoptosis was assayed by fluorescence microscopy. RESULTS: HEMA or TEGDMA exposure resulted in ROS formation and concentration-dependent apoptosis as well as phosphorylation of ERK. Phosphorylation of JNK and p38 was induced by HEMA. Selective inhibitors of ERK and JNK modified the apoptotic response after HEMA and TEGDMA exposure, whereas p38 inhibition modified the apoptotic response only after HEMA exposure. Vitamin C reduced HEMA-induced apoptosis. SIGNIFICANCE: ROS formation and differential MAP kinase activation appear to be involved in the apoptotic response following exposure to HEMA and TEGDMA.

Animals↗

Evaluation of silver methenamine method for nanoleakage.

OBJECTIVES: The aim of this study was to evaluate nanoleakage patterns following silver methenamine staining of restorations bonded with a total-etch single bottle system, a self-etching primer system and a total-etch single bottle system after collagen depletion. METHODS: The dentin bonding systems used in this study were Prime and bond 2.1 (PB) and Clearfil SE Bond (CSEB). Cavities were made in grounded labial surfaces of 15 extracted bovine lower incisors, randomly divided into 3 Groups. Group 1 (PB), Group 2 (CSEB) and Group 3 (PB/SH) PB after collagen depletion with sodium hypochlorite (SH). The specimens were restored, sectioned and submitted to silver methenamine staining, polished and observed with low-vacuum back-scattered SEM. One way ANOVA and multiple-comparison Tukey's test were used for statistical analysis of the leakage scores. RESULTS: PB presented significantly greater silver deposition and a distinct pattern when compared to CSEB. No silver deposition was detected for PB after collagen depletion. SIGNIFICANCE: The dentine bonding systems tested were unable to prevent nanoleakage when used according to the manufacturers' instructions; however, CSEB presented a lower level of silver deposition. Collagen depletion prior to PB application may prevent nanoleakage occurrence in dentine walls. Silver methenamine staining may be a useful method for detection of nanoleakage in dentine when the collagen fibrils remain exposed within the hybrid layers.

Acetone↗

The bonding of composite resin to moist enamel.

OBJECTIVE: To determine the effect on the bond strength of modern dentine bonding agents to etched enamel of surface contamination with water. DESIGN: Fifteen bond strength measurements were made for bonds prepared to both moist and dry etched enamel for each of three test and one control materials. RESULTS: For two materials (Scotchbond 1 and Prime and Bond 2.1) the bond strength was not affected by the presence of water on the etched enamel surface. A mean bond strength in excess of 25 MPa was achieved for both materials under all conditions. One material (Optibond Solo) showed a 30% increase in bond strength when bonds were formed under wet condition (21.10 MPa compared with 15.35 MPa). The bond strength of the control material, a conventional unfilled bonding resin, decreased markedly with aqueous contamination (9.14 MPa compared with 26.75 MPa). CONCLUSION: Etched enamel should be rehydrated routinely prior to bonding composite resin to its surface using a water displacing dentine bonding system.

Acid Etching, Dental↗

The influence of fiber reinforcement of composites on shear bond strengths to enamel.

STATEMENT OF PROBLEM: Fiber-reinforced composites (FRC) are used in direct intra-oral applications as periodontal splints and chairside tooth replacement by bonding them to etched enamel with resin adhesives and composites. There is little information regarding the effect of FRC on the shear bond strength of composite to etched enamel. PURPOSE: The purpose of this study was to examine the effect of resin preimpregnated and non-preimpregnated fiber-reinforced composites on enamel to composite shear bond strength (SBS). MATERIAL AND METHODS: Specimen groups (n = 12) consisted of a control (composite with no fiber reinforcement), Ribbond, Splint-It Unidirectional, Splint-It Woven, and Connect, which were bonded to 37% phosphoric acid etched Prime and Bond NT adhesive-treated bovine enamel surfaces on a bed of Tetric Flow composite. Specimens were thermocycled 1000 times between 5 degrees and 55 degrees C and loaded on a universal testing machine in shear at a linear increasing load until fracture (MPa). The fractured surfaces of the debonded specimens were evaluated to determine the nature of the fracture with a light binocular microscope (x10). Shear bond strength data were subjected to analysis of variance (ANOVA) and Student-Newman-Kuels tests (P <.05). RESULTS: Mean MPa +/- SD for the test groups were as follows: Control, 15.6 +/- 2.4; Splint-It Unidirectional, 15.3 +/- 2.4; Splint-It Woven, 16.5 +/- 1.8; Connect, 18.8 +/- 1.5; and Ribbond, 15.8 +/- 2.2. The Connect FRC group had significantly higher (P <0.05) enamel SBS than all other groups. Fracture analysis showed varying types of failures among the groups, with cohesive fractures within the fiber reinforcement of Splint-It Unidirectional and Connect, cohesive fractures within the bonding resin/flowable composite for Ribbond and the control, and adhesive fracture at the fiber reinforcement interface with Splint-It Woven. CONCLUSION: Within the limitations of this study, no differences in SBS were observed with the addition of 3 of the 4 FRCs compared to composite without FRC, with the exception of the Connect product which provided significantly higher SBS values.

Acid Etching, Dental↗

A new method for sealing composite resin contraction gaps in lined cavities.

Composite resin restorations are often applied in cavities where cervical margins are left unetched, resulting in poorer adaptation in this area. Recent experiments have indicated the possibility of impregnating with resin the gap caused by polymerization contraction. Cavities were prepared in vitro and in vivo. A thin liner was applied inside and outside the cavity. Except for the cervical wall, enamel margins were bevelled and acid-etched, and the cavities restored with Concise Enamel Bond and Composite. In another series, cavities with unetched enamel were restored. Since the liner was placed outside the cavity margins, excess material could be removed without blockage of the air-filled gap. Enamel Bond with a fluorescent additive was applied to various margins. Ground sections were prepared, and the penetration of this resin into the gap was examined with a microscope. In most teeth, the resin penetrated from 0.5 to 2 mm from the cervical margins. Similar penetration was seen from unetched margins, except for the occlusal one. No penetration was seen at acid-etched margins. By impregnating gaps with low-viscous resin after the filling has cured, one can obtain an improved seal at unetched margins.

Acid Etching, Dental↗