Hongye Yang

Effects of different artificial ageing methods on the degradation of adhesive-dentine interfaces.

OBJECTIVES To compare the effects of four commonly used artificial ageing methods (water storage, thermocycling, NaOCl storage and pH cycling) on the degradation of adhesive-dentine interfaces. METHODS Fifty molars were sectioned parallel to the occlusal plane, polished and randomly divided into two adhesive groups: An etch-and-rinse adhesive Adper SingleBond 2 and a self-etch adhesive G-Bond. After the composite built up, the specimens from each adhesive group were sectioned into beams, which were then assigned to one of the following groups: Group 1 (control), 24h of water storage; Group 2, 6 months of water storage; Group 3, 10,000 runs of thermocycling; Group 4, 1h of 10% NaOCl storage; and Group 5, 15 runs of pH cycling. The microtensile bond strengths were then tested. The failure modes were classified with a stereomicroscope and representative interface was analyzed with a field-emission scanning electron microscopy (FESEM). Nanoleakage expression was evaluated through FESEM in the backscattered mode. RESULTS The four artificial ageing methods decreased the bonding strength to nearly 50% and increased the nanoleakage expression of both adhesive systems compared with the control treatment. Adhesive failures were the predominant fracture modes in all groups. However, differences in detailed morphology were observed among the different groups. CONCLUSIONS Water storage, thermocycling, NaOCl storage and pH cycling could obtain similar degradation effectiveness through appropriate parameter selection. Each in vitro artificial ageing method had its own mechanisms, characteristics and application scope for degrading the adhesive-dentin interfaces. CLINICAL SIGNIFICANCE Water storage is simple, low-cost but time-consuming; thermocycling lacks of a standard agreement; NaOCl storage is time-saving but mainly degrades the organic phase; pH cycling can resemble cariogenic condition but needs further studies. Researchers focusing on bonding durability studies should be deliberate in selecting an appropriate ageing model based on the differences of test material, purpose and time.

Effect of pretreatment with calcium- containing desensitizer on the dentine bonding of mild self-etch adhesives

Desensitizing agents are frequently applied to sensitive teeth and may affect subsequent resin bonding. The current study aimed to evaluate the bonding performance of two self-etch adhesives containing functional monomers to dentine pretreated with three new calcium-containing desensitizers. No desensitizer was applied in the control group. Groups 1, 2, and 3 were treated with an arginine-calcium carbonate-containing polishing paste, a casein phosphopeptide-amorphous calcium phosphate (CPP-ACP)-containing paste, and an experimental hydroxyapatite paste, respectively. G-Bond and Clearfil S(3) Bond were used for bonding after desensitizer treatments. The microtensile bond strength (μTBS) was tested (n = 20 beams per group) and failure mode distribution was analyzed. Scanning electron microscopy was used to observe the occlusion of dentinal tubules. The mean (±SD) μTBS values, expressed in MPa, of groups 1, 2, and 3 and the control group were, respectively, 30.81 (7.79), 44.41 (8.02), 31.49 (6.13), and 41.40 (8.67) for G-Bond and 39.63 (9.59), 32.55 (7.86), 37.50 (8.60), 27.90 (6.52) for S3 Bond. Most failures were recorded as adhesive failure (69.375%), instead of cohesive failure or mixed failure. The dentinal tubules were seldom plugged in group 2, but were mostly occluded in groups 1 and 3. Two-way anova indicated that desensitizer application in association with a compatible adhesive system should be used when endeavoring to control hypersensitivity without adverse interference in bonding.

Biomimetic Intrafibrillar Mineralization of Type I Collagen with Intermediate Precursors-loaded Mesoporous Carriers

Limited continuous replenishment of the mineralization medium is a restriction for in-situ solution-based remineralization of hypomineralized body tissues. Here, we report a process that generated amine-functionalized mesoporous silica nanoparticles for sustained release of biomimetic analog-stabilized amorphous calcium phosphate precursors. Both two-dimensional and three-dimensional collagen models can be intrafibrillarly mineralized with these released fluidic intermediate precursors. This represents an important advance in the translation of biomineralization concepts into regimes for in-situ remineralization of bone and teeth.

Translation of a solution-based biomineralization concept into a carrier-based delivery system via the use of expanded-pore mesoporous silica

UNLABELLED Mineralization of collagen fibrils using solution-based systems containing biomimetic analogs of matrix proteins to stabilize supersaturated calcium phosphate solutions have been predictably achieved in vitro. Solution-based systems have limitations when used for in-situ remineralization of human hypomineralized tissues because periodic replenishment of the mineralizing solution is infeasible. A carrier-based platform designed for delivering mineral precursors would be highly desirable. In the present work, mesoporous silica nanoparticles with expanded pores (eMSN; 14.8nm) were synthesized. Polyacrylic acid-stabilized amorphous calcium phosphate (PA-ACP) was generated from a supersaturated calcium and phosphate ion-containing solution, and chosen as the model mineralizing phase. After amine functionalization (AF) of the eMSN through a post-grafting method, the positively-charged AF-eMSN enabled loading of PA-ACP by electrostatic interaction. In-vitro cytotoxicity testing indicated that PA-ACP@AF-eMSN was highly biocompatible. The release kinetics of mineralization precursors from PA-ACP@AF-eMSN was characterized by an initial period of rapid calcium and phosphate release that reached a plateau after 120h. Intrafibrillar mineralization was examined using a 2-D fibrillar collagen model; successful mineralization was confirmed using transmission electron microscopy. To date, this is the first endeavor that employs expanded-pore mesoporous silica to deliver polymer-stabilized intermediate precursors of calcium phosphate for intrafibrillar mineralization of collagen. The carrier-based delivery system bridges the gap between contemporary solution-based biomineralization concepts and clinical practice, and is useful for in-situ remineralization of bone and teeth. STATEMENT OF SIGNIFICANCE Concepts of collagen biomineralization have been reasonably well established in the past few years and intrafibrillar mineralization of collagen fibrils can be predictably achieved with analogs of matrix proteins using solution-based systems. However, solution-based systems have their limitations in clinical applications that require direct application of mineralization precursors in-situ because periodic replenishment of the mineralizing solution is impossible. The present work presents for the first time, the use of amine-functionalized mesoporous silica with expanded pores for loading and release of polyacid-stabilized amorphous calcium phosphate mineralization precursors, and for intrafibrillar mineralization of type I collagen fibrils. This strategy represents an important step in the translational application of contemporary biomineralization concepts for in-situ remineralization of bone and teeth.

A novel application of nanohydroxyapatite/mesoporous silica biocomposite on treating dentin hypersensitivity: An in vitro study.

OBJECTIVES To fabricate a nanohydroxyapatite/mesoporous silica nanoparticle (nHAp@MSN) biocomposite and investigate its effectiveness on dentinal tubule occlusion, acid-resistant stability, and microtensile bond strength (MTBS). METHODS The nHAp@MSN biocomposite was synthesized and characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, N2 adsorption-desorption isotherms, field-emission scanning electron microscopy (FESEM), and high-resolution transmission electron microscopy (HRTEM). Thirty-two simulated sensitive dentin discs were prepared and randomly divided into four groups according to the following treatments (n=8 each): Group 1, no treatment; Group 2, NovaMin, 15 s×2; Group 3, MSN, 15 s×2; Group 4, nHAp@MSN, 15 s×2. Then, four discs per group were post-treated with 6wt.% citric acid challenge to test their acid-resistant stability. The effects on dentinal tubule occlusion were observed by FESEM. A self-etch adhesive (G-Bond) was applied to evaluate the MTBS. The cytotoxicity was detected using the Cell Counting Kit-8 (CCK-8) assay. RESULTS Results revealed that the nHAp@MSN biocomposite was successfully fabricated. nHAp@MSN could effectively occlude the dentinal tubules, and the intratubular crystals were tightly associated with the tubular wall. After citric acid attack, nHAp@MSN exhibited the highest acid-resistant stability among the four groups. Moreover, no significant difference in MTBS was noted among the four groups (P>0.05). CCK-8 assay identified that nHAp@MSN induced no more than 20% cell death even at the highest concentration of 640μg/mL. CONCLUSIONS The application of the nHAp@MSN biocomposite resulted in efficient dentinal tubule occlusion, acid-resistant stability, and did not compromise immediate bond strength between dentin and self-etch adhesive system. CLINICAL SIGNIFICANCE The nHAp@MSN biocomposite indicates enormous potential as a new strategy for relieving dentin hypersensitivity.

Effects of the application sequence of calcium-containing desensitising pastes during etch-and-rinse adhesive restoration

OBJECTIVES To evaluate the effects of different application sequence of calcium-containing desensitising pastes on bonding effectiveness and tubule occlusion during etch-and-rinse (E&R) adhesive restoration. METHODS Seventy molars were sectioned parallel to the occlusal plane, polished and randomly divided into seven groups (n=10). Group 1 was etched with 35% phosphoric acid for 15s. Groups 2-4 were treated with different calcium-containing desensitisers, including an arginine-calcium carbonate (Arg-CaCO3)-containing paste, a casein phosphopeptide-amorphous calcium phosphate (CPP-ACP)-containing paste and a calcium-sodium phosphosilicate (Novamin)-containing paste, respectively. Afterward, these groups were etched with 35% phosphoric acid for 15s. Groups 5-7 were initially etched and then treated with Arg-CaCO3-, CPP-ACP- and Novamin-containing desensitisers, respectively. In each group, samples were equally distributed into two subgroups (n=5) to bond with either a two-step E&R adhesive Adper SingleBond 2 (SB) or a three-step E&R adhesive Adper ScotchBond Multi-Purpose (SBMP). The microtensile bond strengths (MTBS) were tested and fracture modes were analyzed by stereomicroscopy and field-emission scanning electron microscopy (FESEM). Eight additional dentine disks were prepared to evaluate tubule occlusion prior to bonding using FESEM. RESULTS The application sequence of calcium-containing desensitising pastes did not significantly affect MTBS irrespective of two-step SB (P>0.05) or three-step SBMP E&R adhesives (P>0.05). Effective dentinal tubule occlusion was observed in the mode of etching-desensitising. CONCLUSIONS Applying calcium-containing desensitisers (particularly Arg-CaCO3- and Novamin-based) after etching during E&R adhesive restoration could achieve effective tubule occlusion without affecting the bonding strength.

Effect of adjunctive application of epigallocatechin-3-gallate and ethanol-wet bonding on adhesive-dentin bonds.

OBJECTIVES To determine the effect of the combined use of epigallocatechin-3-gallate (EGCG) and ethanol-wet bonding (EWB) on resin-dentin bonds. METHODS Sixty molars were sectioned, polished, and randomly divided into six groups (n=10) according to the following pretreatments: group 1, water-wet bonding (WWB); group 2, WWB with 0.02% (w/v) EGCG; group 3, WWB with 0.1% EGCG; group 4, EWB; group 5, EWB with 0.02% EGCG; and group 6, EWB with 0.1% EGCG. An etch-and-rinse adhesive was then used, followed by the resin composites building. The microtensile bond strength (MTBS), failure modes and interfacial nanoleakage were separately determined after 24h water storage or 10,000 runs of thermocycling. RESULTS Both pretreatment method (P<0.05) and thermocycling (P<0.05) significantly influenced bond strength and nanoleakage. Irrespective of thermocycling, the 0.02% EGCG/ethanol (group 5) pretreated adhesive-dentin interfaces showed higher MTBS than the control group (P<0.05). Nanoleakage expression of all groups increased after thermocycling (P<0.05) except group 5. Adhesive failure was the main fracture pattern in all groups. CONCLUSION This study showed that pretreatment with 0.02% EGCG/ethanol solutions can effectively improve immediate bond strength and bond stability of etch-and-rinse adhesives on dentin. CLINICAL SIGNIFICANCE The adjunctive application of EGCG and EWB provides a new strategy for dentists to obtain the desired bond effectiveness during adhesive restoration in clinical practice.

Paucity of Nanolayering in Resin-Dentin Interfaces of MDP-based Adhesives

Self-assembled nanolayering structures have been reported in resin-dentin interfaces created by adhesives that contain 10-methacryloyloxydecyl dihydrogen phosphate (10-MDP). These structures have been hypothesized to contribute to bond durability. The objective of the present study was to determine the extent of nanolayering in resin-dentin interfaces after application of commercialized 10-MDP-containing self-etch and universal adhesives to human dentin. Seven commercialized adhesives were examined: Adhese Universal (Ivoclar-Vivadent), All-Bond Universal (Bisco, Inc.), Clearfil SE Bond 2, Clearfil S3 Bond Plus, Clearfil Universal Bond (all from Kuraray Noritake Dental Inc.), G-Premio Bond (GC Corp.), and Scotchbond Universal (3M ESPE). Each adhesive was applied in the self-etch mode on midcoronal dentin according to the respective manufacturer’s instructions. Bonded specimens (n = 6) were covered with flowable resin composite, processed for transmission electron microscopy, and examined at 30 random sites without staining. Thin-film glancing angle X-ray diffraction (XRD) was used to detect the characteristic peaks exhibited by nanolayering (n = 4). The control consisted of 15%wt, 10%wt, and 5%wt 10-MDP (DM Healthcare Products, Inc.) dissolved in a mixed solvent (ethanol and water weight ratio 9:8, with photoinitiators). Experimental primers were applied to dentin for 20 s, covered with hydrophobic resin layer, and examined in the same manner. Profuse nanolayering with highly ordered periodicity (~3.7 nm wide) was observed adjacent to partially dissolved apatite crystallites in dentin treated with the 15% 10-MDP primer. Three peaks in the 2θ range of 2.40° (3.68 nm), 4.78° (1.85 nm), and 7.18° (1.23 nm) were identified from thin-film XRD. Reduction in the extent of nanolayering was observed in the 10% and 5% 10-MDP experimental primer-dentin interface along with lower intensity XRD peaks. Nanolayering and characteristic XRD peaks were rarely observed in specimens prepared from the commercialized adhesives. The sparsity of nanolayering in resin-dentin interfaces created by commercialized adhesives challenges its clinical effectiveness as a mechanism for improving bond longevity in dentin bonding.

Effect of silane pretreatment on the immediate bonding of universal adhesives to computer-aided design/computer-aided manufacturing lithium disilicate glass ceramics

The aim of this study was to investigate the effect of silane pretreatment on the universal adhesive bonding between lithium disilicate glass ceramic and composite resin. IPS e.max ceramic blocks etched with hydrofluoric acid were randomly assigned to one of eight groups treated with one of four universal adhesives (two silane-free adhesives and two silane-containing adhesives), each with or without silane pretreatment. Bonded specimens were stored in water for 24 h. The shear bond strength (SBS) of the ceramic-resin interface was measured to evaluate bond strength, and the debonded interface after the SBS test was analysed using field-emission scanning electron microscopy to determine failure mode. Light microscopy was performed to analyse microleakage and marginal sealing ability. Silane pretreatment significantly and positively influenced SBS and marginal sealing ability. For all the universal adhesive groups, SBS increased and the percentage of microleakage decreased after the pretreatment. Without the pretreatment, SBS and the percentage of microleakage were not significantly different between the silane-containing universal adhesive groups and the silane-free groups. Cohesive failure was the main fracture pattern. The results suggest that additional silane pretreatment can effectively improve the bonding strength and marginal sealing of adhesives to lithium disilicate glass ceramics. The bonding performance of silane-containing universal adhesives without pretreatment is similar to that of silane-free adhesives.

Effect of chemical interaction on the bonding strengths of self-etching adhesives to deproteinised dentine

OBJECTIVES The present study examined (1) the chemical interaction between three self-etching adhesives and sodium hypochlorite (NaOCl)-deproteinised dentine, and (2) the influence of NaOCl treatment on bond strength of self-etching adhesives with/without adhesive functional monomers to dentine. METHODS Caries-free dentine disks (control) and those treated with 5.25% NaOCl for 60s were prepared. Xeno V (no functional monomers), G-Bond (containing 4-MET) or S3 Bond (containing 10-MDP) were applied to the NaOCl-treated dentine and either left without further treatment, or rinsed with 100% ethanol or distilled water. Attenuated total reflection (ATR) spectroscopy and field-emission scanning electron microscopy (FE-SEM) were used to evaluate the affinity of functional monomers with deproteinised dentine. Chemical interaction between the functional monomers and deproteinised dentine was evaluated using thin-film X-ray diffraction (TF-XRD). Microtensile bond strength (MTBS) was used to evaluate the mechanical property of the adhesives, either immediately or after thermo-cycling (5-55°C) for 10,000 cycles. RESULTS According to the ATR and FE-SEM results, G-Bond and S3 Bond showed stronger affinity to deproteinised dentine than Xeno V even after rinsing with water. TF-XRD showed that chemical interaction between S3 Bond and deproteinised dentine occurred by formation of 10-MDP-Ca salt. Both deproteinisation and thermo-cycling adversely affected the MTBS of Xeno V (P<0.05) but deproteinisation had no significant influence on S3 Bond. CONCLUSIONS When bonding to NaOCl-treated dentine, self-etch adhesives containing functional monomers (10-MDP) can maintain immediate and aged bond strengths after 10,000 thermal cycles.