Young Kyung Kim

Critical Review on Methacrylate Resin–based Root Canal Sealers

INTRODUCTION Four generations of methacrylate resin-based sealers have been available commercially. Three of these were introduced during the last 5 years when the concept of simultaneous bonding of root canal sealers to root filling materials and dentin was popularized. METHODS This article presents an overview of methacrylate resin-based sealers, with the objectives of clarifying the behavior of these materials and delineating their limitations in clinical application. RESULTS The first generation sealer was introduced in the mid-1970s. The initial enthusiasm associated with its use eventually diminished as a result of its suboptimal physical, biologic, and clinical properties. With advances in self-etching adhesive technology acquired from adhesive dentistry, methacrylate resin-based sealers were reintroduced in the beginning of the 21st century to support the introduction of bondable root canal filling materials. Three different generations of these sealers have since been available commercially. Although some in vitro studies on the sealing ability, self-etching potential, biocompatibility, and removability of the sealers showed better potential over conventional nonbonding sealers, accomplishing the ideal goal of a monoblock in the root canal space with these materials is still regarded as a major challenge. CONCLUSIONS On the basis of the in vitro and in vivo data available to date, there appears to be no clear benefit with the use of methacrylate resin-based sealers in conjunction with adhesive root filling materials at this point in their development.

Hierarchical and non-hierarchical mineralisation of collagen

Biomineralisation of collagen involves functional motifs incorporated in extracellular matrix protein molecules to accomplish the objectives of stabilising amorphous calcium phosphate into nanoprecursors and directing the nucleation and growth of apatite within collagen fibrils. Here we report the use of small inorganic polyphosphate molecules to template hierarchical intrafibrillar apatite assembly in reconstituted collagen in the presence of polyacrylic acid to sequester calcium and phosphate into transient amorphous nanophases. The use of polyphosphate without a sequestration analogue resulted only in randomly-oriented extrafibrillar precipitations along the fibrillar surface. Conversely, the use of polyacrylic acid without a templating analogue resulted only in non-hierarchical intrafibrillar mineralisation with continuous apatite strands instead of discrete crystallites. The ability of using simple non-protein molecules to recapitulate different levels of structural hierarchy in mineralised collagen signifies the ultimate simplicity in Natures biomineralisation design principles and challenges the need for using more complex recombinant matrix proteins in bioengineering applications.

Effects of different exposure times and concentrations of sodium hypochlorite/ethylenediaminetetraacetic acid on the structural integrity of mineralized dentin.

INTRODUCTION This study tested the null hypothesis that there is no difference between the use of 1.3% NaOCl/17% ethylenediaminetetraacetic acid (EDTA) and 5.25% NaOCl/17% EDTA irrigation regimens on the collagen degradation and flexural strength reduction in mineralized dentin. METHODS Dentin powder and mineralized dentin sections were immersed in 1.3% or 5.25% NaOCl for 10-240 minutes and then rinsed with 17% EDTA as the final irrigant for 2 minutes. Untreated mineralized dentin powder/sections served as controls in the respective experiments. Dentin powders were examined by using Fourier transform infrared (FT-IR) spectroscopy to analyze their relative subsurface intact collagen content with the apatite/collagen ratio. Hydrated dentin sections were subjected to 3-point flexure under water for determining their flexural strengths. RESULTS Collagen degradation was significantly increased and the flexural strength of mineralized dentin was significantly reduced after the use of 5.25% NaOCl as the initial irrigant for more than 1 hour (P < .05). Conversely, changes were insignificant when 1.3% NaOCl was used as the initial irrigant for up to 4 hours (Kruskal-Wallis analysis of variance, n = 10, P < .05). CONCLUSIONS The null hypothesis was rejected. The deleterious effects attributed to the use of NaOCl on dentin are concentration-dependent and time-dependent and are not associated with the demineralization caused by the use of EDTA as the final active irrigant.

Mineralisation of reconstituted collagen using polyvinylphosphonic acid/polyacrylic acid templating matrix protein analogues in the presence of calcium, phosphate and hydroxyl ions

The complex morphologies of mineralised collagen fibrils are regulated through interactions between the collagen matrix and non-collagenous extracellular proteins. In the present study, polyvinylphosphonic acid, a biomimetic analogue of matrix phosphoproteins, was synthesised and confirmed with FTIR and NMR. Biomimetic mineralisation of reconstituted collagen fibrils devoid of natural non-collagenous proteins was demonstrated with TEM using a Portland cement-containing resin composite and a phosphate-containing fluid in the presence of polyacrylic acid as sequestration, and polyvinylphosphonic acid as templating matrix protein analogues. In the presence of these dual biomimetic analogues in the mineralisation medium, intrafibrillar and extrafibrillar mineralisation via bottom-up nanoparticle assembly based on the non-classical crystallisation pathway could be identified. Conversely, only large mineral spheres with no preferred association with collagen fibrils were observed in the absence of biomimetic analogues in the medium. Mineral phases were evident within the collagen fibrils as early as 4 h after the initially-formed amorphous calcium phosphate nanoprecursors were transformed into apatite nanocrystals. Selected area electron diffraction patterns of highly mineralised collagen fibrils were nearly identical to those of natural bone, with apatite crystallites preferentially aligned along the collagen fibril axes.

Shear bond strengths of various luting cements to zirconia ceramic: Surface chemical aspects

OBJECTIVES To measure the shear bond strengths of various luting cements to a sandblasted zirconia ceramic and to determine the surface energy parameters of the luting cements. METHODS Two conventional glass ionomer cements, two resin-modified glass ionomer cements, two compomer cements, and two adhesive resin cements were prepared and bonded to sandblasted zirconia (Lava). All bonded specimens were stored in water at 37°C for 48 h and then half of them additionally thermocycled 10,000 times prior to the shear bond strength test (n=10). Surface roughness (R(a)) values and surface energy parameters of the eight luting cements and polished zirconia ceramic were evaluated using a profilometer and contact angle measurements, respectively (n=10). The bond strength and surface roughness data were statistically analysed using non-parametric and parametric procedures, respectively (α=0.05). Relationships between surface energy parameters and measured shear bond strengths were investigated using the Spearman rank correlation test. RESULTS Panavia F 2.0 and Principle produced higher bond strengths than the other cements, with no significant changes before and after thermocycling. Fuji I, Ketac Cem Easymix, and Ionotite F yielded near-zero or zero values after thermocycling. All debonded specimens showed adhesive failure. Mean R(a) values ranged from 0.104 to 0.167 μm. We found the base (hydrogen bond accepting) components of the luting cements significantly affected the bond strengths both before and after thermocycling. CONCLUSION It is recommended that the surface energy parameters of luting cements be considered in evaluating their adhesive properties with zirconia ceramic.

Functional biomimetic analogs help remineralize apatite-depleted demineralized resin-infiltrated dentin via a bottom–up approach

Natural biominerals are formed through metastable amorphous precursor phases via a bottom-up, nanoparticle-mediated mineralization mechanism. Using an acid-etched human dentin model to create a layer of completely demineralized collagen matrix, a bio-inspired mineralization scheme has been developed based on the use of dual biomimetic analogs. These analogs help to sequester fluidic amorphous calcium phosphate nanoprecursors and function as templates for guiding homogeneous apatite nucleation within the collagen fibrils. By adopting this scheme for remineralizing adhesive resin-bonded, completely demineralized dentin, we have been able to redeposit intrafibrillar and extrafibrillar apatites in completely demineralized collagen matrices that are imperfectly infiltrated by resins. This study utilizes a spectrum of completely and partially demineralized dentin collagen matrices to further validate the necessity for using a biomimetic analog-containing medium for remineralizing resin-infiltrated partially demineralized collagen matrices in which remnant seed crystallites are present. In control specimens in which biomimetic analogs are absent from the remineralization medium, remineralization could only be seen in partially demineralized collagen matrices, probably by epitaxial growth via a top-down crystallization approach. Conversely, in the presence of biomimetic analogs in the remineralization medium, intrafibrillar remineralization of completely demineralized collagen matrices via a bottom-up crystallization mechanism can additionally be identified. The latter is characterized by the transition of intrafibrillar minerals from an inchoate state of continuously braided microfibrillar electron-dense amorphous strands to discrete nanocrystals, and ultimately into larger crystalline platelets within the collagen fibrils. Biomimetic remineralization via dual biomimetic analogs has the potential to be translated into a functional delivery system for salvaging failing resin-dentin bonds.

Immobilization of a phosphonated analog of matrix phosphoproteins within cross-linked collagen as a templating mechanism for biomimetic mineralization

Immobilization of phosphoproteins on a collagen matrix is important for the induction of intrafibrillar apatite mineralization. Unlike phosphate esters, polyphosphonic acid has no reactive sites for covalent binding to collagen amine groups. Binding of poly(vinyl phosphonic acid) (PVPA), a biomimetic templating analog of matrix phosphoproteins, to collagen was found to be electrostatic in nature. Thus, an alternative retention mechanism was designed for immobilization of PVPA on collagen by cross-linking the latter with carbodiimide (EDC). This mechanism is based on the principle of size exclusion entrapment of PVPA molecules within the internal water compartments of collagen. By cross-linking collagen with EDC, a zero length cross-linking agent, the sieving property of collagen is increased, enabling the PVPA to be immobilized within the collagen. The absence of covalent cross-linking between PVPA and collagen was confirmed by Fourier transform infrared spectroscopy. Based on these results, a concentration range for immobilized PVPA to template intrafibrillar apatite deposition was established and validated using a single layer reconstituted type I collagen mineralization model. In the presence of a polyacrylic acid-containing mineralization medium optimal intrafibrillar mineralization of the EDC-cross-linked collagen was achieved using 500 and 1000 μg ml⁻¹ PVPA. The mineralized fibrils exhibited a hierarchical order of intrafibrillar mineral infiltration, as manifested by the appearance of electron-dense periodicity within unstained fibrils. Understanding the basic processes in intrafibrillar mineralization of reconstituted collagen creates opportunities for the design of tissue engineering materials for hard tissue repair and regeneration.

The effect of initial irrigation with two different sodium hypochlorite concentrations on the erosion of instrumented radicular dentin

OBJECTIVE This study evaluated the effects of different NaOCl concentrations and contact times on removal of the organic phase from mineralized dentin with and without the adjunctive use of EDTA, and the effect of NaOCl concentrations on canal wall erosion after the use of EDTA as the final active irrigant. METHODS Dentin powders were immersed in 5.25% or 1.3% NaOCl for different contact periods and then rinsed with 17% EDTA for 2 min. Before and after the use of 17% EDTA as the final rinse, the NaOCl-treated dentin powders were examined using ATR-FT-IR spectroscopy to analyze the relative loss of organic and inorganic components. Scanning (SEM) and transmission electron microscopy (TEM) were used to examine the erosion of instrumented canal walls irrigated with 5.25% NaOCl/EDTA or 1.3% NaOCl/EDTA. RESULTS Compared with 1.3% NaOCl, less intact collagen remained within the subsurface of the mineralized dentin powder after the use of 5.25% NaOCl, irrespective of subsequent rinsing with 17% EDTA. Canal wall erosion was apparent only under SEM when root canals were irrigated 5.25% NaOCl followed by 17% EDTA. Under TEM examination, subsurface erosion extended 10-15 microm beneath the sealer-bonded dentin surface after the use of 5.25% NaOCl for 20 min. CONCLUSION The superficial destructive effect of NaOCl on mineralized dentin is irreversible and is present irrespective of whether EDTA is subsequently employed as the final active irrigant. The EDTA removes the collagen-depleted apatite phase to expose the underlying cause of destruction that is morphologically perceived as canal wall erosion.

Biomimetic remineralization as a progressive dehydration mechanism of collagen matrices--implications in the aging of resin-dentin bonds.

Biomineralization is a dehydration process in which water from the intrafibrillar compartments of collagen fibrils are progressively replaced by apatites. As water is an important element that induces a lack of durability of resin-dentin bonds, this study has examined the use of a biomimetic remineralization strategy as a progressive dehydration mechanism to preserve joint integrity and maintain adhesive strength after ageing. Human dentin surfaces were bonded with dentin adhesives, restored with resin composites and sectioned into sticks containing the adhesive joint. Experimental specimens were aged in a biomimetic analog-containing remineralizing medium and control specimens in simulated body fluid for up to 12 months. Specimens retrieved after the designated periods were examined by transmission electron microscopy for the presence of water-rich regions using a silver tracer and for collagen degradation within the adhesive joints. Tensile testing was performed to determine the potential loss of bond integrity after ageing. Control specimens exhibited severe collagen degradation within the adhesive joint after ageing. Remineralized specimens exhibited progressive dehydration, as manifested by silver tracer reduction and partial remineralization of water-filled microchannels within the adhesive joint, as well as intrafibrillar remineralization of collagen fibrils that were demineralized initially as part of the bonding procedure. Biomimetic remineralization as a progressive dehydration mechanism of water-rich, resin-sparse collagen matrices enables these adhesive joints to resist degradation over a 12-month ageing period, as verified by the conservation of their tensile bond strength. The ability of the proof of concept biomimetic remineralization strategy to prevent bond degradation warrants further development of clinically relevant delivery systems.

A chemical phosphorylation-inspired design for Type I collagen biomimetic remineralization.

OBJECTIVES Type I collagen alone cannot initiate tissue mineralization. Sodium trimetaphosphate (STMP) is frequently employed as a chemical phosphorylating reagent in the food industry. This study examined the feasibility of using STMP as a functional analog of matrix phosphoproteins for biomimetic remineralization of resin-bonded dentin. METHODS Equilibrium adsorption and desorption studies of STMP were performed using demineralized dentin powder (DDP). Interaction between STMP and DDP was examined using Fourier transform-infrared spectroscopy. Based on those results, a bio-inspired mineralization scheme was developed for chemical phosphorylation of acid-etched dentin with STMP, followed by infiltration of the STMP-treated collagen matrix with two etch-and-rinse adhesives. Resin-dentin interfaces were remineralized in a Portland cement-simulated body fluid system, with or without the use of polyacrylic acid (PAA) as a dual biomimetic analog. Remineralized resin-dentin interfaces were examined unstained using transmission electron microscopy. RESULTS Analysis of saturation binding curves revealed the presence of irreversible phosphate group binding sites on the surface of the DDP. FT-IR provided additional evidence of chemical interaction between STMP and DDP, with increased in the peak intensities of the PO and P-O-C stretching modes. Those peaks returned to their original intensities after alkaline phosphatase treatment. Evidence of intrafibrillar apatite formation could be seen in incompletely resin-infiltrated, STMP-phosphorylated collagen matrices only when PAA was present in the SBF. SIGNIFICANCE These results reinforce the importance of PAA for sequestration of amorphous calcium phosphate nanoprecursors in the biomimetic remineralization scheme. They also highlight the role of STMP as a templating analog of dentin matrix phosphoproteins for inducing intrafibrillar remineralization of apatite nanocrystals within the collagen matrix of incompletely resin-infiltrated dentin.