Limited interaction of a self-adhesive flowable composite with dentin/enamel characterized by TEM.

OBJECTIVES: A new category of composite which does not require any acid etching or bonding protocol prior to application has been introduced. The purpose of this study was to characterize the interfacial ultra-structure at enamel and dentin surfaces by means of transmission electron microscopy (TEM). METHODS: Non-carious human third molars were randomly divided into 6 groups (bur-cut dentin, SiC-ground dentin, fractured dentin, bur-cut enamel, SiC-ground enamel, and un-cut enamel). After preparation of the respective surfaces, the self-adhesive flowable composite (Vertise Flow, Kerr) was applied. Non-demineralized/demineralized and non-stained/stained sections of 70-90nm were prepared following common TEM-specimen processing procedures. Additional specimens were immersed in an ammoniacal silver nitrate solution. RESULTS: The composite-dentin interface was free of voids and no de-bonding occurred during specimen preparation. For bur-cut and SiC-ground dentin, no surface demineralization was observed and the smear contained residual hydroxyapatite. On fractured dentin (i.e. without smear interference), a very thin interaction area of 100-200nm without apparent signs of surface demineralization was seen. When the composite was bonded to enamel, a distinct separation between the self-adhesive composite and enamel was present in all three groups. A tight interaction, yet without distinct dissolution of hydroxyapatite, could only be seen in some regions at bur-cut enamel where smear was absent or sparse. Silver nitrate infiltration was associated with the presence of smear. SIGNIFICANCE: The self-adhesive composite showed limited interaction with smear-covered substrates and aprismatic enamel, which explains its inferior diminished bonding capacity in comparison with current adhesives.

Interfacial fracture toughness of aged adhesive-dentin interfaces.

OBJECTIVE: To assess interfacial fracture toughness of different adhesive approaches and compare to a standard micro-tensile bond-strength (µTBS) test after 6 months water storage. METHODS: Chevron-notched beam fracture toughness (CNB) was determined using a modified ISO 24370:2005 standard. Adhesive-dentin micro-specimens (1.0 mm × 1.0 mm × 8-10 mm) were stressed in tensile until failure to determine the micro-tensile bond strength (µTBS). RESULTS: The highest mean µTBS and interfacial fracture toughness were measured for the multi-step adhesives Clearfil SE Bond (Kuraray Noritake) and OptiBond FL (Kerr). While large differences were observed in the bond strength values (from 7.4 to 27.2 MPa) of the one-step self-etch adhesives tested, interfacial fracture toughness was less different (from 0.7 to 1.0 MPam(1/2)). The adhesive with the lowest mean toughness (All-bond Universal, Bisco) had however the highest Weibull reliability, which might be a better parameter in regard to more consistent clinical performance. The self-adhesive composite Vertise Flow (Kerr) scored significantly lower at all levels. SIGNIFICANCE: Although the ranking of the adhesives tested using CNB and µTBS corresponded well, the outcome of CNB appeared more reliable and less variable.

Dentin-smear remains at self-etch adhesive interface.

OBJECTIVE: The bonding potential of 'mild' self-etch adhesives may be compromised due to smear interference, as they may not dissolve/penetrate the smear layer effectively due to their relatively low acidity. We observed that the thickness of the dentin smear layer differed depending on the surface-preparation methodology used. METHODS: The interaction of an (ultra-)mild self-etch adhesive (Clearfil S3 Bond, Kuraray Noritake) with human dentin, prepared either using a medium-grit diamond bur ('thick', clinically relevant smear layer) or 600-grit SiC-paper ('thin' smear layer), or just fractured (smear-free), was evaluated using high-resolution transmission electron microscopy (TEM). Non-demineralized/demineralized 30-100nm interfacial cross-sections were prepared following common TEM-specimen processing and diamond-knife ultra-microtomy. RESULTS: The adhesive did not dissolve the bur-cut, nor the SiC-ground smear layer, but impregnated it. Within this 'resin-smear complex', hydroxyapatite was abundantly present. At fractured dentin, this complex was not present, while the actual layer of interaction of the adhesive was limited to about 100nm. Non-demineralized 'ultra-thin' (30-50nm) sections confirmed the interfacial ultra-structure to differ for the three surface-preparation methods. An electron dense band was consistently disclosed at the adhesive interface, most likely representing the documented chemical interaction of the functional monomer 10-MDP with Ca. SIGNIFICANCE: The dentin surface-preparation method significantly affects the nature of the smear layer and the interaction with the ultra-mild self-etch adhesive.

Effect of standard and neutral-pH peritoneal dialysis solutions upon fibroblasts proliferation.

INTRODUCTION: Continuous exposition of the peritoneal membrane to conventional dialysis solutions is an important risk factor for inducing structural and functional alterations. OBJECTIVE: To compare in vitro mouse fibroblast NIH-3T3 cell viability after exposition to a neutral pH dialysis solution in comparison to cells exposed to a standard solution. METHODS: Experimental study to compare the effects of a conventional standard or a neutral-pH, low-glucose degradation products peritoneal dialysis solution on the viability of exposed fibroblasts in cell culture. Both solutions were tested in all the commercially available glucose concentrations. Cell viability was evaluated with tetrazolium salt colorimetric assay. RESULTS: Fibroblast viability was significantly superior in the neutral pH solution in comparison to control, in all three glucose concentrations (Optical density in nm-means ± SD: 1.5% 0.295 ± 0.047 vs. 0.372 ± 0.042, p < 0.001; 2.3% 0.270 ± 0.036 vs. 0.337 ± 0.051, p < 0.001; 4.25% 0.284 ± 0.037 vs. 0.332 ± 0.032, p < 0.001; control vs. neutral pH respectively, Student t Test). There was no significant difference in cell viability between the three concentrations of glucose when standard solution was used (ANOVA p = 0.218), although cell viability was higher after exposition to neutral pH peritoneal dialysis fluid at 1.5% in comparison to 2.3 and 4.25% glucose concentrations (ANOVA p = 0.008: Bonferroni 1.5% vs. 2.3% p = 0.033, 1.5% vs. 4.25% p = 0.014, 2.3% vs. 4.25% p = 1.00). CONCLUSION: Cell viability was better in neutral pH dialysis solution, especially in the lower glucose concentration. A more physiological pH and lower glucose degradation products may be responsible for such results.

Effect of standard and neutral-pH peritoneal dialysis solutions upon fibroblasts proliferation / Efeito da solução de diálise peritoneal com pH neutro e padrão sobre a proliferação de fibroblastos

Introduction: Continuous exposition of the peritoneal membrane to conventional dialysis solutions is an important risk factor for inducing structural and functional alterations. Objective: To compare in vitro mouse fibroblast NIH-3T3 cell viability after exposition to a neutral pH dialysis solution in comparison to cells exposed to a standard solution. Methods: Experimental study to compare the effects of a conventional standard or a neutral-pH, low-glucose degradation products peritoneal dialysis solution on the viability of exposed fibroblasts in cell culture. Both solutions were tested in all the commercially available glucose concentrations. Cell viability was evaluated with tetrazolium salt colorimetric assay. Results: Fibroblast viability was significantly superior in the neutral pH solution in comparison to control, in all three glucose concentrations (Optical density in nm-means ± SD: 1.5% 0.295 ± 0.047 vs. 0.372 ± 0.042, p < 0.001; 2.3% 0.270 ± 0.036 vs. 0.337 ± 0.051, p < 0.001; 4.25% 0.284 ± 0.037 vs. 0.332 ± 0.032, p < 0.001; control vs. neutral pH respectively, Student t Test). There was no significant difference in cell viability between the three concentrations of glucose when standard solution was used (ANOVA p = 0.218), although cell viability was higher after exposition to neutral pH peritoneal dialysis fluid at 1.5% in comparison to 2.3 and 4.25% glucose concentrations (ANOVA p = 0.008: Bonferroni 1.5% vs. 2.3% p = 0.033, 1.5% vs. 4.25% p = 0.014, 2.3% vs. 4.25% p = 1.00). Conclusion: Cell viability was better in neutral pH dialysis solution, especially in the lower glucose concentration. A more physiological pH and lower glucose degradation products may be responsible for such results. .

Introdução: A exposição contínua da membrana peritoneal a soluções convencionais de diálise é um importante fator de risco para induzir alterações estruturais e funcionais. Objetivo: Comparar a viabilidade in vitro dos fibroblastos NIH-3T3 de camundongo após exposição à solução de diálise com pH neutro com células expostas à solução padrão. Métodos: Estudo experimental; ambas as soluções foram testadas em todas as concentrações de glicose comercialmente disponíveis. A viabilidade celular foi avaliada por ensaio colorimétrico de sal tetrazólio. Resultados: A viabilidade de fibroblastos foi melhor na solução de pH neutro em relação ao controle nas três concentrações de glicose (densidade óptica em nm-médias ± DP: 1,5% 0,295 ± 0,047 vs. 0,372 ± 0,042, p < 0,001; 2,3% 0,270 ± 0,036 vs. 0,337 ± 0,051, p < 0,001; 4,25% 0,284 ± 0,037 vs. 0,332 ± 0,032, p < 0,001; controle vs. pH neutro respectivamente, teste t de Student). Não houve diferença significativa na viabilidade celular entre as três concentrações de glicose quando solução padrão foi utilizada (ANOVA p = 0,218), embora a viabilidade celular tenha sido superior após exposição aos fluidos de diálise peritoneal neutros, pH 1,5% em comparação com 2,3 e 4,25% de concentrações de glicose (ANOVA p = 0,008: Bonferroni 1,5% vs. 2,3% p = 0,033, 1,5% vs. 4,25% p = 0,014, 2,3% vs. 4,25% p = 1,0). Conclusão: A viabilidade celular foi melhor em solução neutra de pH de diálise, especialmente nas menores concentrações de glicose. O pH fisiológico e com menos produtos de degradação de glicose podem ser responsáveis por estes resultados. .

Bonding effectiveness to different chemically pre-treated dental zirconia.

OBJECTIVE: The objective of this study was to evaluate the effect of different chemical pre-treatments on the bond durability to dental zirconia. METHODS: Fully sintered IPS e.max ZirCAD (Ivoclar Vivadent) blocks were subjected to tribochemical silica sandblasting (CoJet, 3M ESPE). The zirconia samples were additionally pre-treated using one of four zirconia primers/adhesives (Clearfil Ceramic Primer, Kuraray Noritake; Monobond Plus, Ivoclar Vivadent; Scotchbond Universal, 3M ESPE; Z-PRIME Plus, Bisco). Finally, two identically pre-treated zirconia blocks were bonded together using composite cement (RelyX Ultimate, 3M ESPE). The specimens were trimmed at the interface to a cylindrical hourglass and stored in distilled water (7 days, 37 °C), after which they were randomly tested as is or subjected to mechanical ageing involving cyclic tensile stress (10 N, 10 Hz, 10,000 cycles). Subsequently, the micro-tensile bond strength was determined, and SEM fractographic analysis performed. RESULTS: Weibull analysis revealed the highest Weibull scale and shape parameters for the 'Clearfil Ceramic Primer/mechanical ageing' combination. Chemical pre-treatment of CoJet (3M ESPE) sandblasted zirconia using Clearfil Ceramic Primer (Kuraray Noritake) and Monobond Plus (Ivoclar Vivadent) revealed a significantly higher bond strength than when Scotchbond Universal (3M ESPE) and Z-PRIME Plus (Bisco) were used. After ageing, Clearfil Ceramic Primer (Kuraray Noritake) revealed the most stable bond durability. CONCLUSION: Combined mechanical/chemical pre-treatment, the latter with either Clearfil Ceramic Primer (Kuraray Noritake) or Monobond Plus (Ivoclar Vivadent), resulted in the most durable bond to zirconia. CLINICAL RELEVANCE: As a standard procedure to durably bond zirconia to tooth tissue, the application of a combined 10-methacryloyloxydecyl dihydrogen phosphate/silane ceramic primer to zirconia is clinically highly recommended.

Fracture toughness versus micro-tensile bond strength testing of adhesive-dentin interfaces.

OBJECTIVE: To assess interfacial fracture toughness of different adhesive approaches and compare to a standard micro-tensile bond-strength (µTBS) test. METHODS: Chevron-notched beam fracture toughness (CNB) was measured following a modified ISO 24370 standard. Composite bars with dimensions of 3.0×4.0×25 mm were prepared, with the adhesive-dentin interface in the middle. At the adhesive-dentin interface, a chevron notch was prepared using a 0.15 mm thin diamond blade mounted in a water-cooled diamond saw. Each specimen was loaded until failure in a 4-point bend test setup and the fracture toughness was calculated according to the ISO specifications. Similarly, adhesive-dentin micro-specimens (1.0×1.0×8-10 mm) were stressed in tensile until failure to determine the µTBS. RESULTS: A positive correlation (r(2)=0.64) was observed between CNB and µTBS, which however was only nearly statistically significant, mainly due to the dissimilar outcome of Scotchbond Universal (3M ESPE). While few µTBS specimens failed at the adhesive-dentin interface, almost all CNB specimens failed interfacially at the notch tip. Weibull moduli for interfacial fracture toughness were much higher than for µTBS (3.8-11.5 versus 2.7-4.8, respectively), especially relevant with regard to early failures. SIGNIFICANCE: Although the ranking of the adhesives on their bonding effectiveness tested using CNB and µTBS corresponded well, the outcome of CNB appeared more reliable and less variable. Fracture toughness measurement is however more laborious and requires specific equipment. The µTBS nevertheless appeared to remain a valid method to assess bonding effectiveness in a versatile way.

Potential smear layer interference with bonding of self-etching adhesives to dentin.

PURPOSE: To evaluate the effect of smear-layer interposition on the bonding effectiveness of self-etching adhesives with different etching potential. MATERIALS AND METHODS: Bur-cut dentin specimens were obtained from 25 human molars after preparation of the dentin surface with a medium-grit diamond bur (bur-cut). An additional 25 molars were fractured at the midcoronal dentin to create a smear-layer-free surface (smear-free dentin). The prepared teeth were assigned to 5 groups, according to the adhesive to be applied: a strong one-step self-etching adhesive (PLP, Adper Prompt L-Pop, 3M ESPE, pH = 0.8); two ultra-mild one-step self-etching adhesives (C3S, Clearfil Tri-S Bond, Kuraray, pH = 2.7; AEB, Adper Easy Bond, 3M ESPE; pH = 2.7 ); as the self-etching control, a mild two-step self-etching adhesive (CSE, Clearfil SE Bond, Kuraray, pH of primer = 1.9); and as the etch-and-rinse control, a three-step etch-and-rinse adhesive (OFL, Optibond FL, Kerr). After composite buildups were made, all specimens were stored in distilled water (24 h/37°C) prior to microtensile bond strength testing (µTBS). The failure mode was determined with a stereomicroscope at 50X magnification. Representative µTBS specimens were processed for analysis in a Feg-SEM. The Kruskal-Wallis test was performed to determine statistical differences (p < 0.05). RESULTS: Except for the strong one-step self-etching adhesive, all other self-etching adhesives (mild and ultramild) revealed a significantly lower bond strength to bur-cut dentin than to smear-free dentin. The etch-and-rinse adhesive presented the highest µTBS, which was not significantly different when bonded to bur-cut or smear-free dentin. Fracture analysis demonstrated a prevalence of adhesive failures for the self-etching adhesives, while OFL revealed more mixed failures. SEM revealed that smear debris remained part of the adhesive interfacial complex produced by the ultra-mild one-step self-etching adhesive C3S when applied on bur-cut dentin. CONCLUSION: Smear debris interferes with the interaction of mild and ultra-mild self-etching adhesives with dentin.

Hydrolytic stability of three-step etch-and-rinse adhesives in occlusal class-I cavities.

OBJECTIVES: A dental adhesive without small and hydrophilic monomers such as 2-hydroxyethyl methacrylate (HEMA) and triethylene glycol dimethacrylate (TEGDMA) would be beneficial in order to avoid contact allergies. However, these monomers are important to increase infiltration and polymerization of the adhesive. Therefore, the purpose of this study was to evaluate the bonding effectiveness and bond durability of a more hydrophobic and biocompatible adhesive as compared to a conventional three-step etch-and-rinse adhesive. METHODS: Sixteen non-carious human third molars were used to determine the micro-tensile bond strength testing (µTBS) and interfacial ultrastructure by transmission electron microscopy (TEM) of the more hydrophobic cmf adhesive system (Saremco) adhesive as compared to the control OptiBond FL (Kerr). RESULTS: The more hydrophobic and biocompatible three-step etch-and-rinse adhesive was able to produce a reasonable short-time bonding effectiveness. In the long term, the collagen fibrils in the hybrid layer were not effectively protected and were prone to hydrolytic degradation. As a result, long-term bonding effectiveness of this novel adhesive was very low. CONCLUSIONS: Application of a more hydrophobic adhesive without altering the application procedure considerably results in a reduced durability of the created bond CLINICAL RELEVANCE: Omitting small and hydrophilic components from the adhesive formulation may impair the durability of your composite restoration.

Bulk-filling of high C-factor posterior cavities: effect on adhesion to cavity-bottom dentin.

OBJECTIVES: To evaluate the effect of bulk-filling high C-factor posterior cavities on adhesion to cavity-bottom dentin. METHODS: A universal flowable composite (G-ænial Universal Flo, GC), a bulk-fill flowable base composite (SDR Posterior Bulk Fill Flowable Base, Dentsply) and a conventional paste-like composite (Z100, 3M ESPE) were bonded (G-ænial Bond, GC) into standardized cavities with different cavity configurations (C-factors), namely C=3.86 (Class-I cavity of 2.5mm deep, bulk-filled), C=5.57 (Class-I cavity of 4mm deep, bulk-filled), C=1.95 (Class-I cavity of 2.5mm deep, filled in three equal layers) and C=0.26 (flat surface). After one-week water storage, the restorations were sectioned in 4 rectangular micro-specimens and subjected to a micro-tensile bond strength (µTBS) test. RESULTS: Highly significant differences were found between pairs of means of the experimental groups (Kruskal-Wallis, p<0.0001). Using the bulk-fill flowable base composite SDR (Dentsply), no significant differences in µTBS were measured among all cavity configurations (p>0.05). Using the universal flowable composite G-ænial Universal Flo (GC) and the conventional paste-like composite Z100 (3M ESPE), the µTBS to cavity-bottom dentin was not significantly different from that of SDR (Dentsply) when the cavities were layer-filled or the flat surface was build up in layers; it was however significantly lower when the Class-I cavities were filled in bulk, irrespective of cavity depth. SIGNIFICANCE: The filling technique and composite type may have a great impact on the adhesion of the composite, in particular in high C-factor cavities. While the bulk-fill flowable base composite provided satisfactory bond strengths regardless of filling technique and cavity depth, adhesion failed when conventional composites were used in bulk.

Bonding effectiveness of self-adhesive composites to dentin and enamel.

UNLABELLED: Self-adhesive composites (SACs) are claimed to bond to tooth substrate without a separate adhesive. Bonding effectiveness data are however still limited. OBJECTIVES: In SubProject 1, the hypothesis was tested that the micro-tensile bond strength (µTBS) to dentin of two flowable SACs was alike that of a one-step self-etch adhesive (1-SEa) combined with a flowable composite (flowC). In SubProject 2, the hypothesis was tested that the nature of the smear layer did not affect the µTBS of the SACs to dentin/enamel. METHODS: SubProject 1: The µTBS to bur-cut dentin of two SACs (Fusio Liquid Dentin, Pentron; Vertise Flow, Kerr) was measured and compared to that of four 1-SEa/flowC combinations (AdheSe One/Tetric EvoFlow, Ivoclar Vivadent; Adper Prompt L-Pop/Filtek Supreme XT Flowable, 3M ESPE; iBond/Venus flow, Heraeus Kulzer; Xeno V/X-flow, Dentsply) and of one 3-step etch-and-rinse adhesive (3-E&Ra: OptiBond FL, Kerr) combined with Premise Flowable (Kerr). The effect of pre-etching dentin with phosphoric acid on the µTBS of the SAC Vertise Flow (Kerr) was measured as well. SubProject 2: The µTBS of the two SACs and one 1-SEa/flowC combination (Adper Prompt L-Pop/Filtek Supreme XT Flowable, 3M ESPE) to either bur-cut or SiC-paper ground dentin/enamel was measured. The effect of pre-etching enamel with phosphoric acid on the µTBS of the SAC Vertise Flow (Kerr) was also measured. RESULTS: SubProject 1: The µTBS to dentin of both SACs was significantly lower than that of the 1-SEa/flowC and the 3-E&Ra/flowC combinations, of which the latter performed best. The SAC Fusio Liquid Dentin (Pentron) bonded significantly better to dentin than Vertise Flow (Kerr), except when dentin had additionally been pre-etched with phosphoric acid. SubProject 2: Surface smear did not interfere with bonding of the SACs to dentin/enamel, while their µTBS remained significantly lower than that of the 1-SEa/flowC combination. Prior phosphoric-acid etching of dentin/enamel significantly ameliorated the bonding effectiveness of Vertise Flow (Kerr). SIGNIFICANCE: The bonding effectiveness of flowable SACs underscores that of 1-SEa's and one 'gold-standard' 3-E&Ra when combined with their proprietary flowable composite. Consequently, routine clinical application of SACs should be carefully considered.

Effect of low-shrinking composite on the bonding effectiveness of two adhesives in occlusal Class-I cavities.

The purpose of this study was to evaluate if a low-shrinking composite can improve the bonding effectiveness of adhesives in highly constrained conditions. A low-shrinking composite ('els-extra low shrinkage', Saremco) was bonded in standardized occlusal Class-I cavities using a three-step ('cmf', Saremco) and a two-step etch-and-rinse adhesive ('XP Bond', Dentsply). Both adhesives were also combined with a conventional composite ('Z100', 3M ESPE). Half of the restored cavities were exposed to 20,000 thermo-cycles. 3-way ANOVA revealed a significant effect for the factors 'adhesive' and 'composite' (both p<0.0001), but not for 'thermo-cycling' (p=0.994). Significantly higher bond strengths were recorded for the low-shrinking composite than for the control composite, using either of the adhesives. The low-shrinking composite in combination with the three-step etch-and-rinse adhesive performed best in the high C-factor Class-I cavity. The two-step etch-and-rinse adhesive suffered strongly from polymerization-shrinkage stress, which could be partially restored by using the low-shrinking composite.

A 13-year clinical evaluation of two three-step etch-and-rinse adhesives in non-carious class-V lesions.

This 13-year randomized clinical trial compared the clinical effectiveness of two three-step etch-and-rinse adhesives in combination with a hybrid, stiffer composite versus a micro-filled, more flexible composite. The influence of composite stiffness on the clinical performance of one of the adhesives was assessed as well. One hundred and forty-two non-carious cervical lesions were restored with composites with contrasting stiffness. Seventy-one patients randomly received two cervical restorations placed following two out of three adhesive procedures: (1) the three-step etch-and-rinse adhesive Permaquick applied with the stiff micro-hybrid composite Amelogen Hybrid (PMQ-H, Ultradent), (2) Permaquick applied with the more flexible micro-filled Amelogen Microfill (PMQ-M, Ultradent), or (3) the "gold-standard" three-step etch-and-rinse adhesive Optibond FL applied with the micro-hybrid composite Prodigy (OFL-P, Kerr). The restorations were evaluated after 6 months, 1, 2, 3, 5, 7, and 13 years of clinical service regarding their retention, marginal integrity and discoloration, caries occurrence, preservation of tooth vitality, and post-operative sensitivity. Retention loss, severe marginal defects, and/or discoloration that needed intervention (repair or replacement) and the occurrence of caries were considered as clinical failures. The recall rate at 13 years was 77%. Bond degradation after 13 years was mainly characterized by a further increase in the presence of small but clinically acceptable marginal defects and superficial marginal discoloration. Twelve percent of the OFL-P restorations were clinically unacceptable. In the PMQ group, 22% of the PMQ-M restorations and 26% of the PMQ-H restorations needed repair or replacement. Regarding the clinical failure rate, Optibond FL scored significantly better than Permaquick (McNemar; p = 0.015). No statistically significant differences were found between the micro-filled and the hybrid composite for each of the parameters evaluated (McNemar, p > 0.05). After 13 years of clinical functioning, the clinical effectiveness of the three adhesive/composite combinations remained highly acceptable.

Effect of dentin location and long-term water storage on bonding effectiveness of dentin adhesives.

Dentin is a variable substrate with properties that change considerable in a single surface. The purpose of this study was to evaluate the bonding effectiveness to these different dentin locations and evaluate these differences over time. After bonding procedures with five different adhesives, small micro-tensile bond strength (µTBS) beams were prepared and dichotomously divided in 'center' and 'periphery' dentin specimens. After 1 week, 3, 6 and 12 months of water storage the µTBS of specimens of each group was determined, enabling a paired study design. The bond strengths of both etch&rinse adhesives were insensitive to regional variability. For the two-step self-etch adhesives, a marked increase in bond strengths was observed with increasing amount of intertubular dentin. Regional variability did not affect the long-term bonding effectiveness for any of the adhesives tested. In conclusion, only for the mild self-etch adhesives, µTBS to 'periphery' dentin was higher than for the 'center' specimens.

Enzymatic degradation of adhesive-dentin interfaces produced by mild self-etch adhesives.

Endogenous matrix metalloproteinases (MMPs) released by adhesive procedures may degrade collagen in the hybrid layer and so compromise the bonding effectiveness of etch-and-rinse adhesives. In this study, endogenous enzymatic degradation was evaluated for several simplified self-etch adhesives. In addition, primers were modified by adding two MMP inhibitors: chlorhexidine, a commonly used disinfectant, but also a non-specific MMP inhibitor; and SB-3CT, a specific inhibitor of MMP-2 and MMP-9. Gelatin zymography of fresh human dentin powder was used to identify the enzymes released by the adhesives. Micro-tensile bond strength (µTBS) testing was used to assess the mechanical properties of resin-dentin interfaces over time. In none of the experimental groups treated with the mild self-etch adhesives was MMP-2 and/or MMP-9 identified. Also, no difference in the µTBS was measured for the inhibitor-modified and the control inhibitor-free adhesives after 6 months of water storage. It is concluded that in contrast to etch-and-rinse adhesives, the involvement of endogenous MMP-2 and MMP-9 in the bond-degradation process is minimal for mild self-etch adhesives.

Dynamic versus static bond-strength testing of adhesive interfaces.

UNLABELLED: A static bond-strength test is often regarded as clinically less relevant, since such abrupt loading of the adhesive-tooth bond clinically never occurs. Therefore, dynamic fatigue testing is often claimed to better predict the clinical effectiveness of adhesives. OBJECTIVES: To measure the micro-tensile fatigue resistance (µTFR) of adhesives bonded to dentin, and to compare their µTFR to their micro-tensile bond strength (µTBS). METHODS: The bonding effectiveness (including fracture analysis) of three adhesives (OptiBond FL, Kerr: 3-step etch-and-rinse adhesive or 3-E&Ra; Clearfil SE, Kuraray: 2-step self-etch adhesive or 2-SEa; G-Bond, GC: 1-step self-etch adhesive or 1-SEa) was measured by means of both a dynamic µTFR and a static µTBS approach. Preparation and test set-up of the micro-specimens were identical for both tests. In fatigue, specimens were tested with a wide range of selected loads at 2Hz and at 10Hz until failure, or until 10(4) cycles were reached. At 2Hz, the µTFR was also measured after 3-month water storage. The µTFR was determined using a logistic regression model. Two-way ANOVA and Tukey HSD multiple comparisons test were used to determine statistical differences in µTBS. RESULTS: The 1-SEa recorded significantly lower values in µTFR at 10Hz and in µTBS than the 2-SEa and 3-E&Ra. The 1-SEa and the 2-SEa performed significantly lower in µTFR than the 3-E&Ra, when tested at 2Hz after 3-month water storage. Fatigue testing at 2Hz after 1-week water storage did not reveal any differences in µTFR between the three adhesives. SIGNIFICANCE: The 3-E&Ra performed best in terms of bonding effectiveness, irrespective of the experimental condition or test used. The µTBS test proved once more to be a reliable laboratory test in ranking contemporary adhesives on their bonding effectiveness.

Two-year clinical evaluation of a self-adhesive luting agent for ceramic inlays.

PURPOSE: The aim of this prospective randomized controlled clinical trial was to evaluate the 2-year clinical performance of a self-adhesive resin cement, RelyX Unicem (3M ESPE), used for cementation of ceramic inlays. In addition, the influence of selectively acid etching enamel prior to luting on marginal integrity, inlay integrity, tooth integrity, sensitivity, and complications of the restored teeth was assessed. The hypothesis tested was that there was no significant difference in these criteria between restorations with (Etch) or without prior enamel acid etching (Non-etch). MATERIALS AND METHODS: Sixty-two IPS Empress 2 inlays/onlays were placed in 31 patients by two experienced clinicians. The restorations were luted with RelyX Unicem with (=experimental group; Etch) or without (=control group; Non-etch) prior enamel etching with phosphoric acid. At baseline, 6 months, 1 year and 2 years after placement, the restorations were assessed by two calibrated investigators using modified USPHS criteria. RESULTS: The recall rate at 24 months was 96.6%. Two restorations were clinically unacceptable due to loss of retention, leading to a survival rate of 96.6% (Kaplan-Meier). No significant difference was noted between the experimental group and the control group regarding marginal integrity, inlay integrity, tooth integrity, complications and sensitivity (McNemar, p > 0.05). An obvious deterioration in marginal adaptation was observed after 24 months as only 21.7% (Etch = 23.4%; Non-etch = 20%) of the restorations exhibited an excellent marginal adaptation compared to 70.7% (Etch = 75%; Non-etch = 66.7%) at baseline. In 74.9% of the restorations, small, still clinically acceptable marginal deficiencies were observed (Etch = 76.6%; Non-etch = 73.2%). CONCLUSION: The self-adhesive resin cement RelyX Unicem showed acceptable clinical behavior after two years of clinical service. Selective enamel etching prior to luting had no significant influence on marginal integrity, inlay integrity, tooth integrity, sensitivity or complications of the restored teeth after 24 months. Longer term evaluation is needed to confirm this finding.

Bonding effectiveness of two contemporary self-etch adhesives to enamel and dentin.

OBJECTIVES: Among contemporary adhesives, self-etch adhesives have been adopted by general practitioners for routine adhesive restorative purposes, mainly because of their ease of use. However, many versions that differ for their clinical application procedure, pH, number of components, etc., are currently available on the market. The purpose of this study was to determine the bonding effectiveness of two new self-etch adhesives (Adper Easy Bond and Adper ScotchBond SE, 3M ESPE) to enamel and dentin using a micro-tensile bond strength (microTBS) protocol and to characterise the interfacial ultra-structure at enamel and dentin using transmission electron microscopy (TEM). METHODS: The adhesives were applied onto coronal human enamel and dentin surfaces and built up with the micro-hybrid resin composite Z100 (3M ESPE). The 'gold-standard' two-step self-etch adhesive Clearfil SE Bond (Kuraray) served as control. Specimens were sectioned to sticks and trimmed at the interface to a cylindrical hour-glass shape ('trimmed' micro-specimens). Non-demineralized and demineralized TEM sections through the adhesive-dentin/enamel interface were prepared by ultra-microtomy. RESULTS: The microTBS of the two self-etch adhesives to enamel was statistically significantly lower than that of the control. To dentin, the microTBS of Adper Easy Bond was significantly lower than that of Adper ScotchBond SE and the control. TEM showed a tight interface to enamel for all three self-etch adhesives. A relatively thick, completely demineralized and acid-resistant hybrid layer was formed at dentin by Adper ScotchBond SE, whereas the interaction of Adper Easy Bond was much shallower, and comparable to that of so-called 'ultra-mild' self-etch adhesives. Some degree of spot- and cluster-like nano-leakage was observed for both adhesives, but did not differ in extent and form from that observed for the control. CONCLUSIONS: Although the new two self-etch adhesives revealed a tight interaction at both enamel and dentin, their bond strength to both tooth tissues was generally lower than that of the control adhesive. Nevertheless, their bonding effectiveness appears in line with other simplified self-etch adhesives.

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.

Bonding effectiveness and interfacial characterization of a HEMA/TEGDMA-free three-step etch&rinse adhesive.

OBJECTIVES: Small and hydrophilic monomers as HEMA and TEGDMA can easily penetrate human tissues. For biocompatibility issues it is therefore better to avoid such monomers in dental adhesive formulations. The purpose of this study was (1) to determine the micro-tensile bond strength (muTBS) to enamel/dentin of a HEMA/TEGDMA-free three-step etch&rinse adhesive (cmf Adhesive System, Saremco), and (2) to characterize it's interfacial interaction with enamel/dentin using transmission electron microscopy (TEM). METHODS: Twelve intact freshly extracted human third molars were used for muTBS. The three-step etch&rinse adhesive OptiBond FL (Kerr) served as control adhesive. After bonding procedures and subsequent composite build-up (Z100, 3M ESPE), specimens were sectioned to sticks and trimmed at the interface to a cylindrical hour-glass shape. TEM section of non-demineralized and demineralized sections were prepared by ultra-microtomy and examined. RESULTS: The muTBS of the cmf Adhesive System to enamel was not statistically significantly different from that of the control (OptiBond FL) adhesive (p=0.3512); the muTBS to dentin was however significantly lower (p<0.0001). TEM showed a tight interface at enamel for both adhesives. A relatively thick, completely demineralized and acid-resistant hybrid layer was formed at dentin. Some degree of spot- and cluster-like nano-leakage was observed with cmf Adhesive System, but did not differ in extent and form in comparison to that observed with the OptiBond FL control. CONCLUSIONS: The new three-step adhesive cmf Adhesive System showed indications of good bonding effectiveness, certainly to enamel and only significantly lower to dentin, when compared to the gold-standard adhesive. The latter may be related to the adapted HEMA/TEGDMA-free formulation and the somewhat lower mechanical properties.