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Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique

Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique http://jap.or.kr J Adv Prosthodont 2013;5:226-33 http://dx.doi.org/10.4047/jap.2013.5.3.226 Adhesion of 10-MDP containing resin cements to dentin with and without the etch- and-rinse technique 1 1 1 Volkan Turp *, DDS, PhD, Deniz Sen , DDS, PhD, Betul Tuncelli , DDS, PhD, Mutlu Özcan , DDS, DMD, PhD University of Istanbul, Faculty of Dentistry, Department of Prosthodontics, Istanbul, Turkey University of Zurich, Dental Materials Unit, Center for Dental and Oral Medicine, Clinic for Fixed and Removable Prosthodontics and Dental Materials Science, Zurich, Switzerland PURPOSE. This study evaluated the adhesion of 10-MDP containing self-etch and self-adhesive resin cements to dentin with and without the use of etch-and-rinse technique. MATERIALS AND METHODS. Human third molars (N=180) were randomly divided into 6 groups (n=30 per group). Conventional (Panavia F2.0, Kuraray-PAN) and self-adhesive resin cements (Clearfil SA, Kuraray-CSA) were bonded to dentin surfaces either after application of 3-step etch-and-rinse (35% H PO + ED Primer) or two-step self-etch adhesive resin (Clearfil SE Bond). 3 4 Specimens were subjected to shear bond strength test using the universal testing machine (0.5 mm/min). The failure types were analyzed using a stereomicroscope and quality of hybrid layer was observed under a scanning electron microscope. The data (MPa) were analyzed using two-way ANOVA and Tukey’s tests (α=.05). RESULTS. Overall, PAN adhesive cement showed significantly higher mean bond strength (12.5 ± 2.3 - 14.1 ± 2.4 MPa) than CSA cement (9.3 ± 1.4 - 13.9 ± 1.9 MPa) (P<.001). Adhesive failures were more frequent in CSA cement groups when used in conjunction with two-step self-adhesive (68%) or no adhesive at all (66%). Hybrid layer quality was inferior in CSA compared to PAN cement in all conditions. CONCLUSION. In clinical situations where bonding to dentin substrate is crucial, both conventional and self-adhesive resin cements based on 10-MDP can benefit from etch-and-rinse technique to achieve better quality of adhesion in the early clinical period. [ J Adv Prosthodont 2013;5:226-33] KEY WORDS: Adhesion; Bond strength; Dentin; Hybrid layer; Self-adhesive cement chanical retention between the resin cement and the dentin INTRODUCTION tubuli takes place when the adhesive resin penetrates into the intratubular and intertubular dentin, forming resin tags The adhesion mechanism of resin cements to dental tissues and the hybrid layer. Micromechanical interlocking is the and especially to dentin, has been studied thoroughly in the most important adhesion mechanism of resin to dentin. last few decades. The establishment of effective microme- However, several factors such as acid-etching, moisture condition of the tooth, penetration depth of adhesive resin Corresponding author: into dentin and dentin depth can affect the formation of Volkan Turp hybrid layer and resin tags. Department of Prosthodontics, Faculty of Dentistry, University of Istanbul, 34093 Fatih Istanbul, Turkey The dentin bonding mechanism is essentially based on Tel. 905353521632: e-mail, vturp@istanbul.edu.tr the infiltration of resin monomers into the porosities creat- Received December 6, 2012 / Last Revision July 16, 2013 / Accepted August 7, 2013 ed by removal of mineral or inorganic material from the dental tissues. This exchange results in micro-mechanical © 2013 The Korean Academy of Prosthodontics 3,4 This is an Open Access article distributed under the terms of the Creative interlocking in the porosities formed. Successful dentin Commons Attribution Non-Commercial License (http://creativecommons. bonding could be achieved through several routes. The so- org/licenses/by-nc/3.0) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original called “etch-and-rinse” technique is the conventional three- work is properly cited. step adhesion procedure. The tooth substrate is first etched 226 Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique with 30-40% phosphoric acid (H PO ) and then rinsed off. of 2.0 mm thickness from the occlusal surfaces of the teeth 3 4 Following acid etching, adhesive resin is applied on the were removed by means of a slow-speed diamond saw conditioned tooth surface. For dentin, the bonding mecha- (Isomet, Buehler Ltd. Lake Bluff, IL, USA) under water- nism of etch-and-rinse adhesives primarily depends on cooling to expose flat deep dentin surfaces. Standardization micro-mechanical retention of resin with the exposed colla- of smear layer was achieved by grinding the dentin surfaces gen fibrils. For enamel, total etch technique is the most with 600 grit silicon carbide paper. effective and reliable method for long-term clinical success. The adhesive systems were applied according to the In the “self-etch” approach, adhesives condition and manufacturers’ instructions. Application procedures and prime dentin are applied at the same time, and no rinsing is product information is displayed in Table 1. A transparent required. In this procedure the clinical application time is polyethylene mold (diameter: 4 mm and height: 6 mm) was shortened and technique sensitivity is significantly reduced. used to bond the resin cements onto dentin surfaces (Fig. Self-etch adhesives can be categorized as “mild” and 1A). “strong”. Strong self-etch adhesives with functional mono- In Group 1, conventional adhesive resin cement mers have low pH (<1) and their bonding mechanism is (Panavia F 2.0, Kuraray, Tokyo, Japan) (PAN) was applied reported to be similar to etch-and-rinse adhesives. ‘Mild’ following etch-and-rinse and bonding (ED Primer, self-etch adhesives (pH≈2) selectively demineralize the den- Kuraray). In Group 2, PAN resin cement was applied fol- tin surface and are reported to form a shallow hybrid layer. lowing bonding (ED Primer) without acid etching. In Adhesion is ensured by chemical interaction between resid- Group 3, self-adhesive resin cement (Clearfil SA, Kuraray) ual hydroxyapatite and functional monomers. (CSA) was applied following etch-and-rinse and bonding Several self-etching adhesive systems contain specific (Clearfil SE, Kuraray). In Group 4, CSA resin cement was functional monomers which enhance the performance of applied following bonding (Clearfil SE) without acid etch- adhesion. The functional monomers may help conditioning ing. In Group 5, only CSA resin cement was applied onto dental tissues, increase monomer penetration, and also dentin surfaces neither with acid etching nor bonding. Lastly, in Group 6, only PAN resin cement was applied improve the chemical adhesion to hard tissues of the onto dentin surfaces neither with acid etching nor bonding. tooth. 10-methacryloyloxydecyl dihydrogen phosphate (10- MDP) is one of the most commonly used functional Light activation was performed for 20 seconds, using a monomers; it is the hydrophilic phosphate monomer that quartz tungsten halogen curing device (Hilux 200, increases resin diffusion and adhesion by causing acidic Benlioglu, Ankara Turkey) with irradiance of 600 mW/cm . decalcification and binding to calcium ions or amino The specimens were stored for 24 hours in dark at room groups of tooth structure. It is reported to be one of the temperature prior to bond strength tests. most successful materials in the market for chemical bond- 11,12 ing. On the other hand, self-adhesive cements do not Bonding strength was evaluated using a mechanical require conditioning the dentin or ceramic surfaces. Such shear test. Specimens were placed firmly in the universal testing machine (Shimadzu AG-IS, Shimadzu, Kyoto, Japan) cements have multifunctional phosphoric acid dimethacry- late modified monomers. However, their diffusion level and the shear force was applied until fracture of the speci- 12-17 into dentin and their hydrolytic stability are not optimal. men (Fig. 1B). The load was applied at the dentin/adhesive Adhesion to deeper tooth substrates with contemporary interface, as close to the surface of the tooth as possible. A strong adhesives is an interesting subject which is not stud- crosshead speed of 0.5 mm/min was used for loading. ied thoroughly in the literature. The objectives of this study Subsequently, specimens were evaluated under optical were to evaluate the adhesion of two different 10-MDP microscope (Leica M80, Leica Microsystems, Wetzlar, containing adhesive resin cements to deep dentin using Germany) at ×40 magnification in order to investigate the either etch-and-rinse or two-step self-etch bonding tech- mode of failure. The types of failures were categorized as; niques and analyze the failure types. The null hypothesis adhesive failure between tooth and resin cement (A), cohe- tested was that adhesion of 10-MDP containing resin sive failure of resin cement (C) or mixed failure where resin cements would not show difference when used in combina- cement was failed partially cohesively and partially adhe- tion with etch-and-rinse or two-step self-etch system. sively on the specimen (M). The specimens were sectioned longitudinally and inter- MATERIALS AND METHODS faces were wet polished with silicone carbide papers of This study was approved by the Ethics Research Committee #600, #1000, #1200 grit in sequence. Following polishing, of Istanbul University Faculty of Medicine (Istanbul the interfaces were decalcified (37% H PO for 10 seconds) 3 4 University, Istanbul, Turkey) (Approval no: 2013/317). and deproteinized (2% NaOCl solution for 1 minute) in Intact human third molars without caries (N=180) were order to evaluate the hybrid layer. used for this study. The roots of the teeth were embedded The hybrid layer and surface pattern were investigated in auto-polymerized acrylic resin (Takilon, SPD Salmoiraghi for all experimental groups using scanning electron micros- Produzione Dentaria S.r.l Mulazzano, Italy) and randomly copy (SEM) (JSM 7000F, JEOL, Japan) by selecting one divided into 6 groups (n=30 per group). Dental materials specimen with bonding strength closest to mean value of The Journal of Advanced Prosthodontics 227 J Adv Prosthodont 2013;5:226-33 Table 1. Brands, manufacturers, chemical compositions and application protocols of the materials used in the study Manufacturer Material Composition Application (Lot No.) Paste A: Bis-GMA; TEGDMA; 10-MDP; Hydrophobic aromatic dimethacrylate; silanated barium glass filler; silanated colloidal silica; Auto-mix cement; apply onto Kuraray Co, dI-camphorquinone; benzoyl peroxide; initiator. the sample surface using Clearfil SA Cement Osaka, Japan Paste B: Bis-GMA; Hydrophobic aromatic dimethacrylate; teflon mold; light polymerize (00857A) Hydrophobic aliphatic dimethacrylate; silanated barium glass filler; for 40 s. silanated colloidal silica; surface treated sodium fluoride; accelerators; pigments. Primer: 10-MDP; Hydrophilic Dimetacrilate; di-camphorquinone; N,N- Apply primer for 20 s. Kuraray Co, diethanol-p-toludine; water. Dry gently with air. Clearfil SE Bond Osaka, Japan Adhesive: 10-MDP; bis-GMA; HEMA; hydrophobic dimetacrylate; Apply adhesive; apply air (00606A) dI-camphorquinone; N,N-diethanol-p-toludine; silanated colloidal gently, light polymerize for silica. 10 s. Paste A: 10-Methacryloyloxydecyl dihydrogen phosphate; Hydrophobic aromatic dimethacrylate; Hydrophobic aliphatic Mix equal amounts of Paste dimethacrylate; Hydrophilic aliphatic dimethacrylate; Silanated silica Kuraray Co, A and B for 20 s.; apply onto filler; Silanated colloidal silica; l-Camphorquinone; Catalysts; Initiators Panavia F 2.0 Osaka, Japan the sample surface using Paste B: sodium fluoride; Hydrophobic aromatic dimethacrylate; (41174) teflon mold; light polymerize Hydrophobic aliphatic dimethacrylate; Hydrophilic aliphatic for 40 s. dimethacrylate; Silanated barium glass filler; Catalysts; Accelerators; Pigments; Others Kuraray Co, Mix equal amounts of liquid A Liquid A: 2-hydroxyethyl methacrylate; 10-Methacryloyloxydecyl Osaka Japan and B, dihydrogen phosphate; N-Methacryloyl-5-aminosalicylic acid; Water; (Primer A - Apply the mixture for 20 s. ED Primer Accelerators 00222A) Remove excess liquid with Liquid B: N-Methacryloyl-5-aminosalicylic acid; Water; (Primer B - gentle air stream. Catalysts; Accelerators 00101B) Light polymerize for 10 s. Prime Dent H PO conditioning for 15 s. 3 4 Total Etch Illinois, USA 35% Phosphoric Acid, fumared silica Rinse with water for 10 s. (HF29M) Leave teeth moist. A B Fig. 1. (A) schematic diagram of specimen and (B) the shear testing. 228 Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique the group. The specimens were covered with a thin layer of did not significantly increase the bond strength of CSA platinum (Sputter-coated) for SEM observation. The whole cement when compared to direct application (9.3 ± 1.4 fractured surface at the dentin side was observed under the MPa) (P>.05). Similarly, for the PAN adhesive cement the SEM. bond strength did not differ significantly between bond- ing(12.5 ± 2.3 MPa) and direct applications (12.8 ± 2.6 Statistical analysis was performed using SPSS 11.0 soft- MPa) (P>.05). ware for Windows (SPSS Inc., Chicago, IL, USA). The Adhesive failures were more frequent in CSA cement assumptions of normality and equal variances across groups when used in conjunction with two-step self-adhe- groups were validated. Bond strength data (MPa) were sub- sive (68%) or no adhesive at all (66%) compared to other mitted to analysis of variance (two-way ANOVA). Multiple groups (37-43%) (Table 3). Generally, specimens with lower comparisons were made with Tukey's post-hoc test (α=.05) bond strengths failed to bond adhesively. with the shear bond strength as the dependent and adhe- SEM observations demonstrated well-defined hybrid sion protocols and the cement types as the independent layer with visible resin tags in dentin in PAN cement group factors. P values less than .05 were considered to be statisti- on 35% H P O conditioned dentin and ver y minor 3 4 cally significant in all tests. detached areas were also evident at the interface (Fig. 2). The unconditioned dentin specimens presented thinner hybrid layer and less frequent distribution of resin tags (Fig. RESULTS 3). Overall, PAN adhesive cement showed significantly higher Hybrid layer quality was inferior in CSA compared to mean bond strength (12.5 ± 2.3 - 14.1 ± 2.4 MPa) than PAN cement in all conditions. On CSA specimens, resin CSA cement (9.3 ± 1.4 - 13.9 ± 1.9 MPa) (P<.001) (Table tags were also visible on both H PO conditioned and 3 4 2). Etching dentin with 35% H P O increased bond unconditioned dentin surfaces (Fig. 4, Fig. 5 and Fig. 6). 3 4 strength significantly for both PAN (14.1 ± 2.4 MPa) and Although resin tag formation was present, resin cement showed detached areas from dentin (Fig. 4). On uncondi- CSA (13.8 ± 1.9 MPa) compared to the application of two- step self-etch adhesive resin (12.5 ± 2.3 - 9.8 ± 1.6 MPa, tioned dentin surfaces a superficial interaction and a thin respectively) (P<.05). hybrid layer formation was apparent compared to PAN Application of bonding agent on dentin (9.8 ± 1.6 MPa) (Fig. 7). Table 2. Mean shear bond strengths (MPa) for each group. Results of the post-hoc tests are indicated by superscripted letters. Groups labelled with different superscripted letters are significantly different (P<.05) Group Bond strength (MPa) Panavia F 2.0 + acid etching + bonding 14.1 ± 2.4 Panavia F 2.0 + bonding 12.5 ± 2.3 Clearfil SA Cement + acid etching + bonding 13.8 ± 1.9 Clearfil SA Cement + bonding 9.8 ± 1.6 Clearfil SA Cement 9.3 ± 1.4 Panavia F 2.0 12.8 ± 2.6 Table 3. Percentage distribution of failure modes per group (A: Adhesive, C: Cohesive, M: Mixed) Group A C M Panavia F 2.0 + acid etching + bonding 37 63 0 Panavia F 2.0 + bonding 41 59 0 Clearfil SA Cement + acid etching + bonding 43 53 4 Clearfil SA Cement + bonding 68 27 5 Clearfil SA Cement 66 33 1 Panavia F 2.0 38 60 2 The Journal of Advanced Prosthodontics 229 J Adv Prosthodont 2013;5:226-33 Fig. 2. SEM micrograph of cement-dentin interface luted Fig. 3. SEM micrograph of cement-dentin interface luted with Panavia F2.0 and bonding on unconditioned dentin, with Panavia F2.0 and bonded on etched and rinsed dentin, where a thick hybrid layer (1) and uniform where hybrid layer is thinner compared to acid conditioned group of the same material (1). Also resin distribution of resin tags (2) are visible observed. (Group 1) (×1,000 magnification). tags are weak (2) and are not infused into dentin tubules homogenously (3) (Group 2) (×1,000 magnification). Fig. 4. SEM micrograph of cement-dentin interface luted Fig. 5. SEM micrograph of cement-dentin interface luted with Clearfil SA cement and bonding on etched and with Clearfil SA cement bonded on unconditioned rinsed dentin, where irregular hybrid layer (1) and resin dentin, where hybrid layer is very thin and not present in tag formations (2) are observed (Group 3) (×1,000 some areas (1), resin tags are very few (2) and dentin magnification). tubules are mostly empty (3) (Group 4) (×1000 magnification). 230 Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique Fig. 6. SEM micrograph of cement-dentin interface luted Fig. 7. SEM micrograph of cement-dentin interface luted with Clearfil SA cement on unconditioned dentin, where with Panavia F2.0 cement on unconditioned dentin, hybrid layer is almost not present (1) and number of resin adhesive failure can be observed (Group 6) (×1000 tags are very few in number (2) with empty dentin magnification). tubules (3) (Group 5) (×1000 magnification). were less frequent and more irregular. DISCUSSION CSA resin cement used in this study has self-adhesive Self-etch adhesive resins are easy to use and their shorter properties. Self-adhesive resin cements etch and prime the chair-time presents advantages. On the contrary, etch-and- dentin surface simultaneously without a need for acid appli- rinse systems are more technique sensitive and require cation. However, the bond strength results achieved in the 6,7 experience from clinicians. Since the use of self-etch current study displayed that H PO etching prior to the 3 4 adhesive system resulted in inferior bond results with both application of resin cement positively influences the bond PAN and CSA compared to total etch system on dentin, the strength of self-adhesive cement. It should also be noted null hypothesis was rejected. that self-adhesive resin cements are reported to only inter- Total etch adhesive systems are reported to have better act with superficial dentin, without any presence of a 18 23,24 clinical results on the long term. Resin cement adhesion to hybrid layer or resin tags. This was observed apparent in dentin depends on surface energy of the dentin and the the SEM images. On the unconditioned dentin, the hybrid wettability of the resin cement on the dentin. H PO appli- layer was not present and the resin tags were irregular and 3 4 cation removes the smear layer and increases surface rough- less in number. In addition, detachment of resin tags was ness and thereby, the wettability of the adhesive resin or the observed in some areas. However, H PO etched dentin 3 4 resin cement. It is also speculated that the water content displayed more frequent resin tags and less detached layers. of the dentin increases after acid etching which eventually Similar results with self-adhesive resin cements were report- 23,24 helps the ionization of the acidic monomers in resin ed in previous studies. De Munck et al. reported low 20-22 cements. This results in improved bonding penetration demineralization effect on RelyX Unicem, even on dentin 20-22 23 and more effective surface conditioning. Similarly, in the surfaces without smear layer. Pisani-Proença et al. con- present study, with etch-and-rinse technique, better results firmed that the SEM observations of untreated dentin were achieved compared to self-etch adhesive for both res- shows the need for further improvement for better infiltra- in cements. Microscopy evaluations supported these find- tion and chemical binding of the self-adhesive cements. ings. For the PAN resin cement, H PO etching prior to They also reported that H PO etching of the dentin 3 4 3 4 bonding displayed higher mean bond strength. In the SEM increases the bonding effectiveness of self-adhesive resin observations, application of PAN to H PO conditioned cements. 3 4 dentin surfaces resulted in visible hybrid layer, regular resin It should also be stressed that both PAN and CSA resin tags and no detached layers. Application of the same resin cements demonstrated significantly higher mean bond cement to unconditioned dentin after self-etching adhesive strength when etch-and-rinse technique was used, being less did not have major visual differences in SEM observations, effective for the latter. One reason for this could be attrib- but thickness of the hybrid layer was lower and resin tags uted to the differences in the structure of the hybrid layers. The Journal of Advanced Prosthodontics 231 J Adv Prosthodont 2013;5:226-33 SEM micrographs of PAN cement applied dentin displayed consider this especially in situations where adhesion is tak- a thicker and attached hybrid layer on etched and rinsed ing place mostly to dentin tissues, such as large inlay or dentin. On the other hand, CSA cement applied dentin onlay restorations and excessively prepared teeth for fixed showed thinner hybrid layer and detached local areas. 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The Journal of Advanced Prosthodontics 233 http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png The Journal of Advanced Prosthodontics Pubmed Central

Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique

The Journal of Advanced Prosthodontics , Volume 5 (3) – Aug 31, 2013

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© 2013 The Korean Academy of Prosthodontics
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2005-7806
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2005-7814
DOI
10.4047/jap.2013.5.3.226
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Abstract

http://jap.or.kr J Adv Prosthodont 2013;5:226-33 http://dx.doi.org/10.4047/jap.2013.5.3.226 Adhesion of 10-MDP containing resin cements to dentin with and without the etch- and-rinse technique 1 1 1 Volkan Turp *, DDS, PhD, Deniz Sen , DDS, PhD, Betul Tuncelli , DDS, PhD, Mutlu Özcan , DDS, DMD, PhD University of Istanbul, Faculty of Dentistry, Department of Prosthodontics, Istanbul, Turkey University of Zurich, Dental Materials Unit, Center for Dental and Oral Medicine, Clinic for Fixed and Removable Prosthodontics and Dental Materials Science, Zurich, Switzerland PURPOSE. This study evaluated the adhesion of 10-MDP containing self-etch and self-adhesive resin cements to dentin with and without the use of etch-and-rinse technique. MATERIALS AND METHODS. Human third molars (N=180) were randomly divided into 6 groups (n=30 per group). Conventional (Panavia F2.0, Kuraray-PAN) and self-adhesive resin cements (Clearfil SA, Kuraray-CSA) were bonded to dentin surfaces either after application of 3-step etch-and-rinse (35% H PO + ED Primer) or two-step self-etch adhesive resin (Clearfil SE Bond). 3 4 Specimens were subjected to shear bond strength test using the universal testing machine (0.5 mm/min). The failure types were analyzed using a stereomicroscope and quality of hybrid layer was observed under a scanning electron microscope. The data (MPa) were analyzed using two-way ANOVA and Tukey’s tests (α=.05). RESULTS. Overall, PAN adhesive cement showed significantly higher mean bond strength (12.5 ± 2.3 - 14.1 ± 2.4 MPa) than CSA cement (9.3 ± 1.4 - 13.9 ± 1.9 MPa) (P<.001). Adhesive failures were more frequent in CSA cement groups when used in conjunction with two-step self-adhesive (68%) or no adhesive at all (66%). Hybrid layer quality was inferior in CSA compared to PAN cement in all conditions. CONCLUSION. In clinical situations where bonding to dentin substrate is crucial, both conventional and self-adhesive resin cements based on 10-MDP can benefit from etch-and-rinse technique to achieve better quality of adhesion in the early clinical period. [ J Adv Prosthodont 2013;5:226-33] KEY WORDS: Adhesion; Bond strength; Dentin; Hybrid layer; Self-adhesive cement chanical retention between the resin cement and the dentin INTRODUCTION tubuli takes place when the adhesive resin penetrates into the intratubular and intertubular dentin, forming resin tags The adhesion mechanism of resin cements to dental tissues and the hybrid layer. Micromechanical interlocking is the and especially to dentin, has been studied thoroughly in the most important adhesion mechanism of resin to dentin. last few decades. The establishment of effective microme- However, several factors such as acid-etching, moisture condition of the tooth, penetration depth of adhesive resin Corresponding author: into dentin and dentin depth can affect the formation of Volkan Turp hybrid layer and resin tags. Department of Prosthodontics, Faculty of Dentistry, University of Istanbul, 34093 Fatih Istanbul, Turkey The dentin bonding mechanism is essentially based on Tel. 905353521632: e-mail, vturp@istanbul.edu.tr the infiltration of resin monomers into the porosities creat- Received December 6, 2012 / Last Revision July 16, 2013 / Accepted August 7, 2013 ed by removal of mineral or inorganic material from the dental tissues. This exchange results in micro-mechanical © 2013 The Korean Academy of Prosthodontics 3,4 This is an Open Access article distributed under the terms of the Creative interlocking in the porosities formed. Successful dentin Commons Attribution Non-Commercial License (http://creativecommons. bonding could be achieved through several routes. The so- org/licenses/by-nc/3.0) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original called “etch-and-rinse” technique is the conventional three- work is properly cited. step adhesion procedure. The tooth substrate is first etched 226 Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique with 30-40% phosphoric acid (H PO ) and then rinsed off. of 2.0 mm thickness from the occlusal surfaces of the teeth 3 4 Following acid etching, adhesive resin is applied on the were removed by means of a slow-speed diamond saw conditioned tooth surface. For dentin, the bonding mecha- (Isomet, Buehler Ltd. Lake Bluff, IL, USA) under water- nism of etch-and-rinse adhesives primarily depends on cooling to expose flat deep dentin surfaces. Standardization micro-mechanical retention of resin with the exposed colla- of smear layer was achieved by grinding the dentin surfaces gen fibrils. For enamel, total etch technique is the most with 600 grit silicon carbide paper. effective and reliable method for long-term clinical success. The adhesive systems were applied according to the In the “self-etch” approach, adhesives condition and manufacturers’ instructions. Application procedures and prime dentin are applied at the same time, and no rinsing is product information is displayed in Table 1. A transparent required. In this procedure the clinical application time is polyethylene mold (diameter: 4 mm and height: 6 mm) was shortened and technique sensitivity is significantly reduced. used to bond the resin cements onto dentin surfaces (Fig. Self-etch adhesives can be categorized as “mild” and 1A). “strong”. Strong self-etch adhesives with functional mono- In Group 1, conventional adhesive resin cement mers have low pH (<1) and their bonding mechanism is (Panavia F 2.0, Kuraray, Tokyo, Japan) (PAN) was applied reported to be similar to etch-and-rinse adhesives. ‘Mild’ following etch-and-rinse and bonding (ED Primer, self-etch adhesives (pH≈2) selectively demineralize the den- Kuraray). In Group 2, PAN resin cement was applied fol- tin surface and are reported to form a shallow hybrid layer. lowing bonding (ED Primer) without acid etching. In Adhesion is ensured by chemical interaction between resid- Group 3, self-adhesive resin cement (Clearfil SA, Kuraray) ual hydroxyapatite and functional monomers. (CSA) was applied following etch-and-rinse and bonding Several self-etching adhesive systems contain specific (Clearfil SE, Kuraray). In Group 4, CSA resin cement was functional monomers which enhance the performance of applied following bonding (Clearfil SE) without acid etch- adhesion. The functional monomers may help conditioning ing. In Group 5, only CSA resin cement was applied onto dental tissues, increase monomer penetration, and also dentin surfaces neither with acid etching nor bonding. Lastly, in Group 6, only PAN resin cement was applied improve the chemical adhesion to hard tissues of the onto dentin surfaces neither with acid etching nor bonding. tooth. 10-methacryloyloxydecyl dihydrogen phosphate (10- MDP) is one of the most commonly used functional Light activation was performed for 20 seconds, using a monomers; it is the hydrophilic phosphate monomer that quartz tungsten halogen curing device (Hilux 200, increases resin diffusion and adhesion by causing acidic Benlioglu, Ankara Turkey) with irradiance of 600 mW/cm . decalcification and binding to calcium ions or amino The specimens were stored for 24 hours in dark at room groups of tooth structure. It is reported to be one of the temperature prior to bond strength tests. most successful materials in the market for chemical bond- 11,12 ing. On the other hand, self-adhesive cements do not Bonding strength was evaluated using a mechanical require conditioning the dentin or ceramic surfaces. Such shear test. Specimens were placed firmly in the universal testing machine (Shimadzu AG-IS, Shimadzu, Kyoto, Japan) cements have multifunctional phosphoric acid dimethacry- late modified monomers. However, their diffusion level and the shear force was applied until fracture of the speci- 12-17 into dentin and their hydrolytic stability are not optimal. men (Fig. 1B). The load was applied at the dentin/adhesive Adhesion to deeper tooth substrates with contemporary interface, as close to the surface of the tooth as possible. A strong adhesives is an interesting subject which is not stud- crosshead speed of 0.5 mm/min was used for loading. ied thoroughly in the literature. The objectives of this study Subsequently, specimens were evaluated under optical were to evaluate the adhesion of two different 10-MDP microscope (Leica M80, Leica Microsystems, Wetzlar, containing adhesive resin cements to deep dentin using Germany) at ×40 magnification in order to investigate the either etch-and-rinse or two-step self-etch bonding tech- mode of failure. The types of failures were categorized as; niques and analyze the failure types. The null hypothesis adhesive failure between tooth and resin cement (A), cohe- tested was that adhesion of 10-MDP containing resin sive failure of resin cement (C) or mixed failure where resin cements would not show difference when used in combina- cement was failed partially cohesively and partially adhe- tion with etch-and-rinse or two-step self-etch system. sively on the specimen (M). The specimens were sectioned longitudinally and inter- MATERIALS AND METHODS faces were wet polished with silicone carbide papers of This study was approved by the Ethics Research Committee #600, #1000, #1200 grit in sequence. Following polishing, of Istanbul University Faculty of Medicine (Istanbul the interfaces were decalcified (37% H PO for 10 seconds) 3 4 University, Istanbul, Turkey) (Approval no: 2013/317). and deproteinized (2% NaOCl solution for 1 minute) in Intact human third molars without caries (N=180) were order to evaluate the hybrid layer. used for this study. The roots of the teeth were embedded The hybrid layer and surface pattern were investigated in auto-polymerized acrylic resin (Takilon, SPD Salmoiraghi for all experimental groups using scanning electron micros- Produzione Dentaria S.r.l Mulazzano, Italy) and randomly copy (SEM) (JSM 7000F, JEOL, Japan) by selecting one divided into 6 groups (n=30 per group). Dental materials specimen with bonding strength closest to mean value of The Journal of Advanced Prosthodontics 227 J Adv Prosthodont 2013;5:226-33 Table 1. Brands, manufacturers, chemical compositions and application protocols of the materials used in the study Manufacturer Material Composition Application (Lot No.) Paste A: Bis-GMA; TEGDMA; 10-MDP; Hydrophobic aromatic dimethacrylate; silanated barium glass filler; silanated colloidal silica; Auto-mix cement; apply onto Kuraray Co, dI-camphorquinone; benzoyl peroxide; initiator. the sample surface using Clearfil SA Cement Osaka, Japan Paste B: Bis-GMA; Hydrophobic aromatic dimethacrylate; teflon mold; light polymerize (00857A) Hydrophobic aliphatic dimethacrylate; silanated barium glass filler; for 40 s. silanated colloidal silica; surface treated sodium fluoride; accelerators; pigments. Primer: 10-MDP; Hydrophilic Dimetacrilate; di-camphorquinone; N,N- Apply primer for 20 s. Kuraray Co, diethanol-p-toludine; water. Dry gently with air. Clearfil SE Bond Osaka, Japan Adhesive: 10-MDP; bis-GMA; HEMA; hydrophobic dimetacrylate; Apply adhesive; apply air (00606A) dI-camphorquinone; N,N-diethanol-p-toludine; silanated colloidal gently, light polymerize for silica. 10 s. Paste A: 10-Methacryloyloxydecyl dihydrogen phosphate; Hydrophobic aromatic dimethacrylate; Hydrophobic aliphatic Mix equal amounts of Paste dimethacrylate; Hydrophilic aliphatic dimethacrylate; Silanated silica Kuraray Co, A and B for 20 s.; apply onto filler; Silanated colloidal silica; l-Camphorquinone; Catalysts; Initiators Panavia F 2.0 Osaka, Japan the sample surface using Paste B: sodium fluoride; Hydrophobic aromatic dimethacrylate; (41174) teflon mold; light polymerize Hydrophobic aliphatic dimethacrylate; Hydrophilic aliphatic for 40 s. dimethacrylate; Silanated barium glass filler; Catalysts; Accelerators; Pigments; Others Kuraray Co, Mix equal amounts of liquid A Liquid A: 2-hydroxyethyl methacrylate; 10-Methacryloyloxydecyl Osaka Japan and B, dihydrogen phosphate; N-Methacryloyl-5-aminosalicylic acid; Water; (Primer A - Apply the mixture for 20 s. ED Primer Accelerators 00222A) Remove excess liquid with Liquid B: N-Methacryloyl-5-aminosalicylic acid; Water; (Primer B - gentle air stream. Catalysts; Accelerators 00101B) Light polymerize for 10 s. Prime Dent H PO conditioning for 15 s. 3 4 Total Etch Illinois, USA 35% Phosphoric Acid, fumared silica Rinse with water for 10 s. (HF29M) Leave teeth moist. A B Fig. 1. (A) schematic diagram of specimen and (B) the shear testing. 228 Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique the group. The specimens were covered with a thin layer of did not significantly increase the bond strength of CSA platinum (Sputter-coated) for SEM observation. The whole cement when compared to direct application (9.3 ± 1.4 fractured surface at the dentin side was observed under the MPa) (P>.05). Similarly, for the PAN adhesive cement the SEM. bond strength did not differ significantly between bond- ing(12.5 ± 2.3 MPa) and direct applications (12.8 ± 2.6 Statistical analysis was performed using SPSS 11.0 soft- MPa) (P>.05). ware for Windows (SPSS Inc., Chicago, IL, USA). The Adhesive failures were more frequent in CSA cement assumptions of normality and equal variances across groups when used in conjunction with two-step self-adhe- groups were validated. Bond strength data (MPa) were sub- sive (68%) or no adhesive at all (66%) compared to other mitted to analysis of variance (two-way ANOVA). Multiple groups (37-43%) (Table 3). Generally, specimens with lower comparisons were made with Tukey's post-hoc test (α=.05) bond strengths failed to bond adhesively. with the shear bond strength as the dependent and adhe- SEM observations demonstrated well-defined hybrid sion protocols and the cement types as the independent layer with visible resin tags in dentin in PAN cement group factors. P values less than .05 were considered to be statisti- on 35% H P O conditioned dentin and ver y minor 3 4 cally significant in all tests. detached areas were also evident at the interface (Fig. 2). The unconditioned dentin specimens presented thinner hybrid layer and less frequent distribution of resin tags (Fig. RESULTS 3). Overall, PAN adhesive cement showed significantly higher Hybrid layer quality was inferior in CSA compared to mean bond strength (12.5 ± 2.3 - 14.1 ± 2.4 MPa) than PAN cement in all conditions. On CSA specimens, resin CSA cement (9.3 ± 1.4 - 13.9 ± 1.9 MPa) (P<.001) (Table tags were also visible on both H PO conditioned and 3 4 2). Etching dentin with 35% H P O increased bond unconditioned dentin surfaces (Fig. 4, Fig. 5 and Fig. 6). 3 4 strength significantly for both PAN (14.1 ± 2.4 MPa) and Although resin tag formation was present, resin cement showed detached areas from dentin (Fig. 4). On uncondi- CSA (13.8 ± 1.9 MPa) compared to the application of two- step self-etch adhesive resin (12.5 ± 2.3 - 9.8 ± 1.6 MPa, tioned dentin surfaces a superficial interaction and a thin respectively) (P<.05). hybrid layer formation was apparent compared to PAN Application of bonding agent on dentin (9.8 ± 1.6 MPa) (Fig. 7). Table 2. Mean shear bond strengths (MPa) for each group. Results of the post-hoc tests are indicated by superscripted letters. Groups labelled with different superscripted letters are significantly different (P<.05) Group Bond strength (MPa) Panavia F 2.0 + acid etching + bonding 14.1 ± 2.4 Panavia F 2.0 + bonding 12.5 ± 2.3 Clearfil SA Cement + acid etching + bonding 13.8 ± 1.9 Clearfil SA Cement + bonding 9.8 ± 1.6 Clearfil SA Cement 9.3 ± 1.4 Panavia F 2.0 12.8 ± 2.6 Table 3. Percentage distribution of failure modes per group (A: Adhesive, C: Cohesive, M: Mixed) Group A C M Panavia F 2.0 + acid etching + bonding 37 63 0 Panavia F 2.0 + bonding 41 59 0 Clearfil SA Cement + acid etching + bonding 43 53 4 Clearfil SA Cement + bonding 68 27 5 Clearfil SA Cement 66 33 1 Panavia F 2.0 38 60 2 The Journal of Advanced Prosthodontics 229 J Adv Prosthodont 2013;5:226-33 Fig. 2. SEM micrograph of cement-dentin interface luted Fig. 3. SEM micrograph of cement-dentin interface luted with Panavia F2.0 and bonding on unconditioned dentin, with Panavia F2.0 and bonded on etched and rinsed dentin, where a thick hybrid layer (1) and uniform where hybrid layer is thinner compared to acid conditioned group of the same material (1). Also resin distribution of resin tags (2) are visible observed. (Group 1) (×1,000 magnification). tags are weak (2) and are not infused into dentin tubules homogenously (3) (Group 2) (×1,000 magnification). Fig. 4. SEM micrograph of cement-dentin interface luted Fig. 5. SEM micrograph of cement-dentin interface luted with Clearfil SA cement and bonding on etched and with Clearfil SA cement bonded on unconditioned rinsed dentin, where irregular hybrid layer (1) and resin dentin, where hybrid layer is very thin and not present in tag formations (2) are observed (Group 3) (×1,000 some areas (1), resin tags are very few (2) and dentin magnification). tubules are mostly empty (3) (Group 4) (×1000 magnification). 230 Adhesion of 10-MDP containing resin cements to dentin with and without the etch-and-rinse technique Fig. 6. SEM micrograph of cement-dentin interface luted Fig. 7. SEM micrograph of cement-dentin interface luted with Clearfil SA cement on unconditioned dentin, where with Panavia F2.0 cement on unconditioned dentin, hybrid layer is almost not present (1) and number of resin adhesive failure can be observed (Group 6) (×1000 tags are very few in number (2) with empty dentin magnification). tubules (3) (Group 5) (×1000 magnification). were less frequent and more irregular. DISCUSSION CSA resin cement used in this study has self-adhesive Self-etch adhesive resins are easy to use and their shorter properties. Self-adhesive resin cements etch and prime the chair-time presents advantages. On the contrary, etch-and- dentin surface simultaneously without a need for acid appli- rinse systems are more technique sensitive and require cation. However, the bond strength results achieved in the 6,7 experience from clinicians. Since the use of self-etch current study displayed that H PO etching prior to the 3 4 adhesive system resulted in inferior bond results with both application of resin cement positively influences the bond PAN and CSA compared to total etch system on dentin, the strength of self-adhesive cement. It should also be noted null hypothesis was rejected. that self-adhesive resin cements are reported to only inter- Total etch adhesive systems are reported to have better act with superficial dentin, without any presence of a 18 23,24 clinical results on the long term. Resin cement adhesion to hybrid layer or resin tags. This was observed apparent in dentin depends on surface energy of the dentin and the the SEM images. On the unconditioned dentin, the hybrid wettability of the resin cement on the dentin. H PO appli- layer was not present and the resin tags were irregular and 3 4 cation removes the smear layer and increases surface rough- less in number. In addition, detachment of resin tags was ness and thereby, the wettability of the adhesive resin or the observed in some areas. However, H PO etched dentin 3 4 resin cement. It is also speculated that the water content displayed more frequent resin tags and less detached layers. of the dentin increases after acid etching which eventually Similar results with self-adhesive resin cements were report- 23,24 helps the ionization of the acidic monomers in resin ed in previous studies. De Munck et al. reported low 20-22 cements. This results in improved bonding penetration demineralization effect on RelyX Unicem, even on dentin 20-22 23 and more effective surface conditioning. Similarly, in the surfaces without smear layer. Pisani-Proença et al. con- present study, with etch-and-rinse technique, better results firmed that the SEM observations of untreated dentin were achieved compared to self-etch adhesive for both res- shows the need for further improvement for better infiltra- in cements. Microscopy evaluations supported these find- tion and chemical binding of the self-adhesive cements. ings. For the PAN resin cement, H PO etching prior to They also reported that H PO etching of the dentin 3 4 3 4 bonding displayed higher mean bond strength. In the SEM increases the bonding effectiveness of self-adhesive resin observations, application of PAN to H PO conditioned cements. 3 4 dentin surfaces resulted in visible hybrid layer, regular resin It should also be stressed that both PAN and CSA resin tags and no detached layers. Application of the same resin cements demonstrated significantly higher mean bond cement to unconditioned dentin after self-etching adhesive strength when etch-and-rinse technique was used, being less did not have major visual differences in SEM observations, effective for the latter. One reason for this could be attrib- but thickness of the hybrid layer was lower and resin tags uted to the differences in the structure of the hybrid layers. The Journal of Advanced Prosthodontics 231 J Adv Prosthodont 2013;5:226-33 SEM micrographs of PAN cement applied dentin displayed consider this especially in situations where adhesion is tak- a thicker and attached hybrid layer on etched and rinsed ing place mostly to dentin tissues, such as large inlay or dentin. On the other hand, CSA cement applied dentin onlay restorations and excessively prepared teeth for fixed showed thinner hybrid layer and detached local areas. 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The Journal of Advanced Prosthodontics 233

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The Journal of Advanced ProsthodonticsPubmed Central

Published: Aug 31, 2013

References