Shear bond strength of universal adhesive systems to a bioactive dentin substitute (Biodentine ) at different time intervals

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1 Stomatological Dis Sci 2017;1: DOI: / Original Article Stomatological Disease and Science Open Access Sear bond strengt of universal adesive systems to a bioactive dentin substitute (Biodentine ) at different time intervals Sedef Aksoy, Murat Ünal Department of Pediatric Dentistry, Faculty of Dentistry, Cumuriyet University, Sivas, Turkey. Correspondence to: Dr. Murat Ünal, Department of Pediatric Dentistry, Faculty of Dentistry, Cumuriyet University, Sivas, Turkey. gmuratunal@otmail.com How to cite tis article: Aksoy S, Ünal M. Sear bond strengt of universal adesive systems to a bioactive dentin substitute (Biodentine ) at different time intervals. Stomatological Dis Sci 2017;1: Article istory: Received: 17 May 2017 First Decision: 1 Jun 2017 Revised: 13 Jul 2017 Accepted: 14 Jul 2017 Publised: 25 Dec 2017 Key words: Biodentine, compomer, universal adesive systems, sear bond strengt ABSTRACT Aim: Te aim of tis study was to compare te sear bond strengt (SBS) of various adesive systems to a bioactive dentin substitute Biodentine wit different time intervals. Metods: Tree undred and fifty cylindrical acrylic blocks wit a ole (4 mm diameter and 2 mm eigt) were prepared. Te oles were filled wit Biodentine, and te specimens were allocated into 5 main groups according to waiting times (group 1, ; group 2, ; group 3, ; group 4, ; and group 5, ). All specimens were stored at 37 C wit 100% umidity during te waiting time. Ten eac group was divided into 7 subgroups of 10 units eac: subgroup 1, Prime&Bond NT ; subgroup 2, Single Bond Universal (self-etc mode); subgroup 3, Single Bond Universal (etc and rinse mode); subgroup 4, All-Bond Universal (self-etc mode); subgroup 5, All-Bond Universal (etc and rinse mode); subgroup 6, G-aenial Universal Bond (self-etc mode); and subgroup 7, G-aenial Universal Bond (etc-and-rinse mode). After te application of adesive systems, compomer Dyract XP Bond was applied over Biodentine SBSs were measured using a universal testing macine. After te SBS test, te fractured surfaces were exaed under a stereomicroscope at 25 magnification, and te data were analyzed wit Kruskal-Wallis and Mann-Witney U (wit Bonferroni correction) tests. Results: Biodentine exibits lower sear bond strengt values in te groups. No significant differences were observed between self-etc or etc-and-rinse bonding modes. Conclusion: A - waiting period after te mixing of Biodentine could be useful to obtain iger SBS measurements. Also, similar SBS values were observed for te universal adesives regardless of application mode. INTRODUCTION Mineral trioxide aggregate (MTA) as become a material wic attracted attention in vital pulp treatments wit its proper biologic caracteristics and favorable istological/clinical outcomes [1,2]. However, MTA as some critical disadvantages like te long setting time, ig resolution during te setting process, staining potential in dental tissues and is difficult to use despite its favorable properties [3]. New calcium silicate-based cements, including Biodentine, were developed to overcome tese disadvantages. Biodentine contains tri- and dicalcium silicates as Tis is an open access article licensed under te terms of Creative Commons Attribution 4.0 International License (ttps://creativecommons.org/licenses/by/4.0/), wic permits unrestricted use, distribution, and reproduction in any medium, as long as te original autor is credited and te new creations are licensed under te identical terms. Quick Response Code: For reprints contact: service@oaepublis.com 116 Te Autor(s)

2 te main material, calcium carbonate as a filler tat improves its mecanical properties and zirconium dioxide as a radiopacifier [4]. Its liquid component is composed of distilled water, calcium cloride, and a water-soluble polymer. Calcium cloride acts as an accelerator enabling faster setting of te material [5]. Te water-soluble polymer serves to reduce water/cement ratio tat increases te material strengt [6]. Te most important advantages of Biodentine over MTA include ease of use, ig viscosity, sort setting time ( ) and more favorable pysical properties [7]. Biodentine also as more developed antibacterial property and a lower cytotoxic effect [8]. In addition, its microardness, flexural strengt, and compressive strengt are iger tan tose of te oter calcium silicate cements and similar to tat of dentin [9]. Besides te biocompatibility, bioactivity, and reeralization abilities of pulp capping materials, te bond strengt between restorative and pulp capping materials as great importance for te quality of te filling and te success of te restoration. Regular bonding of compomers to pulp capping materials leads to an adesive bond tat can spread stress equally along te wole adesion site [10]. Te current adesive tecnologies tend to simplify bonding procedures, sorten clinical application time, reduce tecnical sensitivity by reducing application steps and tereby provide standardization [11]. Self-etc (SE) adesive systems were produced in order to eliate acid etcing procedure wic is quite a sensitive tecnique []. Tese adesives are easier to use compared to multi-step etc-and-rinse (ER) adesives. Also, tey ave a faster application procedure and require less tecnical sensitivity [,13]. Te SE tecnique enables ease of application and reduces contaation wit saliva troug reducing procedure steps, particularly in cildren wo are difficult to cooperate [14,15]. A new type of SE adesive described as universal, and multi-mode tat may be applied bot in SE and ER modes as been introduced to te market [16]. Manufacturers reported tat te bonding activity was not compromised wen bot adesive tecniques are used and also tese adesive systems could also be used for selective etcing of enamel margins [17]. Tese adesive systems may be used in bot types so as to enable dentists to apply te most proper adesive protocol to te prepared cavity [16]. Te purpose of tis study is to evaluate sear bond strengt using four different adesive systems to Biodentine wic were stored at five different time intervals. METHODS Bond strengt, Biodentine universal adesive Four commercial adesive systems, Prime&Bond NT (PB) (Caulk/Dentsply International Inc., USA), Single Bond Universal (SB) (3M ESPE, USA), All- Bond Universal (AB) (Bisco, USA), G-aenial Bond Universal (GB) (GC Corporation, Japan) were tested in tis study and applied as recommended by te manufacturers. Te materialsused are listed in Table 1. Specimen fabrication A total of 350 acrylic blocks containing a central ole wit a 4-mm diameter and a 2-mm eigt were prepared. Biodentine (Septodent, Saint-Maur-des- Fosses Cedex, France) was mixed according to te manufacturer s instructions and acrylic blocks were filled wit Biodentine [Figure 1]. Ten, te specimens were divided into 5 main groups according to waiting periods: group 1, ; group 2, ; group 3, ; group 4, ; and group 5,. All specimens stored at 37 C wit 100% umidity during te waiting time. Ten eac main group was divided into 7 subgroups of 10 eac: subgroup 1, PB; subgroup 2, SB selfetc mode (SB-SE); subgroup 3, SB etc-and-rinse mode (SB-ER); subgroup 4, AB self-etc mode (AB- SE); subgroup 5, AB etc-and-rinse mode (AB-ER); subgroup 6, GB self-etc mode (GB-SE); subgroup 7, GB etc-and-rinse (GB-ER) mode. In eac group, te corresponding adesive system was applied over Biodentine according to te group s manufacturer s instructions. Following tis, a compomer material (Dyract XP Dentsply DeTrey, Konstanz, Germany) was applied into a cylindrical plastic matrix wit an internal diameter of 2 mm and a eigt of 2 mm. Ligt curing was adistered wit a ligt-emitting diode ligt curing unit (Elipar S 10, 3M ESPE, St. Paul, MN, USA) wit an intensity of 1,200 mw/cm 2 for 20 s. Tis procedure was repeated at,,, and after mixing an additional 70 samples at eac time period, respectively. Sear bond strengt test Te polymerized specimens were stored at 100% relative umidity at 37 C for. For sear bond strengt testing, te specimens were secured in a older placed on te platen of te testing macine and ten seared wit a knife-edge blade on a universal testing macine (LF Plus, LLOYD Instruments, Amatek Inc., UK) at a crossead speed of 1.0 mm/. Te sear bond strengt in MPa was calculated by dividing te peak load at failure wit te specimen surface area. Fracture analysis Te fractured test specimens were exaed under a 117

3 Bond strengt, Biodentine universal adesive Table 1: Cemical composition and application procedure of te tested materials Materials Composition Mode/steps of application Biodentine Septodent, Saint-Maur-des-Fosses Cedex, France (B08918) Powder: Tri-calcium silicate, di-calcium silicate, calcium carbonate and oxide filler, iron oxide, zirconium oxide radiopacifier Liquid: calcium cloride acceleratorydrosoluble polymer water reducing agent Five doses liquid and powder supplied for 30 s wit a mixed amalgamator Dyract XP, Dentsply DeTrey, Konstanz, Germany ( ) UDMA, carboxylic acid modified dimetacrylate, TEGDMA, trimetacrylate resin, camporquinone, etyl-4- dimetylaobenzoate, BHT, UV stabiliser, strontium-aluo-sodiumfluoropospor-silicate glass, igly dispersed silicon dioxide, strontium fluoride, iron oxide and titanium dioxide pigments (average filler size: 0.8, filler volume 47%) Condac 37 (281014) 37% posporic acid deionized water Self-etc stragety Etc-rinse strategy Prime & BondNT (PB), Caulk/Dentsply International Inc., USA ( ) Single Bond Universal (SB), 3 M Espe, St. Paul, MN, USA (533701) All-Bond Universal (AB), Bisco Scaumburg, IL, USA ( ) Di- and trimetacrylate resins Dipentaerytyritol penta acrylate monopospate UDMA Nanofillers Amorpous silicon dioxide Potoinitiators Stabilisers Cetylae ydrofluoride Acetone 10-MDP pospate monomer, Vitrebond copolymer, HEMA, BISGMA, dimetacrylate resins filler, silane, initiators, etanol, water 10-MDP pospate monomer, HEMA, BISGMA, etanol 1. Apply te to te Biodentine and rub it in for 20 s 2. Gently air-dry te adesive for approximately 5 s for tesolvent to evaporate 3. Ligt cure for 10 s 1. Apply etcant for 15 s 2. Rinse for 10 s 3. Scrub adesive for 20 s 4. Air-tin for 5 s 5. Ligt-cure for 10 s 1. Apply etcant for 15 s 2. Rinse for 10 s 3. Air dry 5 s 4. Apply adesive as for te self-etc mode 1. Apply 2 separate coats 1. Apply etcant for 15 s of adesive, scrubbing te 2. Rinse torougly preparation wit a microbrus for 3. Remove excess water s per coat. Do not ligt cure wit absorbent pellet or ig between coats volume suction for 1-2 s 2. Evaporate excess solvent by 4. Apply adesive as for te torougly air-drying wit an air self-etc mode syringe for at least 10 s, tere sould be no visible movement of te material. Te surface sould ave a uniform glossy appearance 3. Ligt cure for 10 s G-aenial Bond (GB), Acetone, dimetacrylate, TEGDMA, 4-MET, 1. Apply using a microbrus GC, Tokyo, Japan ( ) posporic acid ester monomer, silicon 2. Leave undisturbed for 10 s after dioxide, poto initiator te end of application 3. Dry torougly for 5 s wit oil free air under maximum air pressure 4. Ligt-cure for 10 s 1. Apply etcant for 15 s 2. Rinse for 5 s and gently dry 3. Apply adesive as for te self-etc mode stereomicroscope (Stemi DV4: Carl Zeiss, Gottingen, Germany) at a magnification of 25. Specimen fractures were classified as follows: coesive failure exclusively witin Biodentine, coesive failure exclusively witin compomer, te adesive failure tat occurred at te Biodentine -compomer interface; or mixed failure wen two modes of failure appened simultaneously [Figure 2]. Fracture analysis was performed by a single observer wo was completely uninformed about te experimental groups. For te scanning electron microscope (SEM) analyses, samples randomly selected from te and groups of te failure specimens. Te failure surfaces were sputter-coated wit gold using a Sputter Coater, and specimens were analyzed wit a SEM (Zeiss Evo LS10, Oberkocen, Germany). Te significance of te difference between groups wit regard to median sear bond strengt was analyzed wit Mann Witney U test wen tere were two independent groups and te wit Kruskal-Walis test wen tere were more tan two independent groups. A P level of < 0.05 was accepted as statistically significant. However, Bonferroni correction was done in order to control type 1 error in all potential multicomparisons. RESULTS Mean sear bond values and standard deviations are sown in Table 2. Te samples stored for sowed statistically significantly lower sear bond values compared to te oter time periods, except te PB and AB-SE groups. However, tere was no 118

4 Bond strengt, Biodentine universal adesive A B C D Figure 1: Preparation of working samples and application of compomer significant difference between specimens stored,, and. No statistically significant differences were found between all te adesive systems at eac of te 5 time intervals (,,, and ). In addition, statistically significant differences could not be found between SE and ER modes of universal adesive systems [Table 2]. Table 3 sows te fracture modes of te experimental groups. In SEM and stereomicroscope analysis wile more superficial coesive failures were observed in Biodentine in te groups, deeper coesive failures were seen in te groups. Also, te surface failures of specimens stored for were seen to be more irregular and porous; te surface structure Figure 2: Steriomicroscopic imaging of te failure modes. (A) Adesive failurel; (B) superficial coesive failure in Biodentine; (C) deeper coesive failure in Biodentine; (D) mix failure was seen to be more regular and smoot in te groups [Figure 3]. DISCUSSION Biodentine was put on te market in 2010, and it was recommended to be used as a dentin substitute in addition to its use in indications similar to ProRoot MTA (e.g. pulp capping, perforation repair, apexification and as root-end filling) [18]. Biodentine was reported to ave more developed mecanical properties tan ProRoot MTA and Angelus MTA, besides its biocompatibility and sort setting time [19,20]. Te manufacturer states tat setting time of Biodentine is and final restoration may be completed in te same appointment [21]. Biodentine was reported to set in a sorter time tan MTA, as its liquid contains calcium cloride and its powder contains calcium Table 2: Mean sear bond strengt values (MPa) and standard deviations of eac group (n = 10) Prime Bond Single Bond-SE Single Bond-ER All Bond-SE All Bond-ER G-aenial Bond-SE G-aenial Bond-ER P value 9.39 (4.34) (3.58) (2.41) (2.86) (2.71) (2.73) (2.09) (2.71) (2.11) a (3.16) a.58 (1.41) (3.07) c (5.28) c (3.20) c (2.79).71 (1.74) a.98 (3.47) c.36 (2.91) 13. (3.28) c (2.30) c (3.13) c (1.13) (2.81) b (1.71) c.04 (2.).67 (2.88) c (4.01) c (2.38) c (1.97).98 (3.07) a.62 (2.) c.62 (2.36) (2.23) c (2.83) c (3.03) c P value < < < Wen waiting periods kept constant, comparisons between materials Kruskal-Wallis test, according to te Bonferroni correction for P < results was accepted statistically significant; comparisons between waiting periods in materials, Kruskal-Wallis test, according to te Bonferroni correction for P < results was accepted statistically significant; a statistically significant difference vs. (P < 0.001); b statistically significant difference vs. (P = 0.005); c accepted statistically significant differences vs.. SE: self etc mode; ER: etc and rinse mode 119

5 Bond strengt, Biodentine universal adesive A B te manufacturer. C E G Figure 3: Scanning electron micrograps of BD specimens at 4 different magnifications (70 for A and B, 150 for C and D, 500 for E and F, and 5000 for G and H). (A) Superficial coesive failure in Biodentine in te - group; (B) deeper coseive failure in Biodentine int e - group; (C, E and G) irregular and porous structure can be seen in te - group; (D, F and H) more regular and smoot structure can be seen in te - group carbonate. Te role of calcium cloride in sortening setting time may be explained by its accelerating te ydration of te silicates in te powder of Biodentine and penetrating into te pores, tereby pioneering crystallization [22]. Jang et al. [23] reported te setting time of Biodentine as 15. In anoter study [6], te setting time of Biodentine was reported as 45 differently from te time reported by te manufacturer. In tis study, te imum storing time was detered to be for Biodentine in accordance wit te instructions of D F H A limited number of studies are available in te literature about te bond strengt of Biodentine to resin materials. Odabaş et al. [] assessed SBS of a composite to Biodentine in two different time intervals ( and ) and found iger SBS values in te groups. In te present study, a statistically significant difference was observed between and groups, and groups sowed iger sear bond values. Hasem et al. [25] compared te microsear bond strengt of composite resin to Biodentine glass ionomer cement and resin modified glass ionomer cementby using early (0.5, 20 and ) and late (2 weeks, 1 mont, and 6 monts) aging. Tey reported a statistically significant increase in te microsear values of late aging groups compared to early aging groups and te igest microsear values were reported in group. Kaup et al. [26] reported a significant increase in te sear bond values of Biodentine to permanent toot dentin between 2 days and 1 week storage times. Tey reported tat tis result migt be explained by te fact tat te setting reaction of calcium silicate cement may continue for more tan 1 mont. Atabek et al. [27] evaluated te sear bond strengt of a composite to wite MTA wit different time intervals (4,,, and ) and recommended postponing te restorative procedures for after mixing MTA to acieve optimal pysical properties. In our study, te specimens were stored for,,, and and a statistically significant difference was found between and te oter storage times. Differently from MTA, te statistical results of our study support tat of storage time is sufficient for resinbased restoration placed onto Biodentine. Mean SBS values varied between 9.39 and MPa in our study. Altunsoy et al. [28] reported tat te SBSs of X-tra base and Vertise Flow to Biodentine were 1.69 and 1.2 MPa respectively, wic is muc lower tan our results. In tis study, te lowest value was observed in te PB group, and te maximum Table 3: Distribution of failure modes witin groups (n = 10) Total PB SB-SE SB-ER AB-SE AB-ER GB-SE GB-ER Adesive Mix Coesive in Biodentine Coesive in Compomer PB: Prime Bond; SB: Single Bond; AB: All Bond; GB: G-aenial Bond; SE: self etc mode; ER: etc and rinse mode 0

6 value was observed in te GB-SE group. Te igest bond strengt values were obtained wit te GB group, altoug te values were statistically insignificant. Tis result may be associated wit GB s containing acetone as a solvent wic as a iger vapor pressure. Acetone may be easily removed from te adesion surface and may provide iger bond strengt by facilitating monomer diffusion due to its ig vapor pressure [27]. Lower sear bond strengt was detected in groups wit PB, anoter acetonecontaining adesive system, compared to te oter groups. We note tat ig molecular weigt monomers like uretane dimetacrylate and dipenta erytritol penta acrylate monopospate in composition of PB ave led to a decrease in bond strengt values troug reducing te diffusion capacity of te adesive [29]. Applying adesive systems in eiter SE or ER was seen not to ave a statistically significant effect on bond strengt in te present study. Tis result is similar to te results of te study of Hanabusa et al. [16], Marcesi et al. [17], and Cen et al. [30], wo also reported tat using SE or ER tecnique does not statistically significantly influence bond strengt. Hasem et al. [25] reported tat similar bond strengt values between SE and ER modes migt be due to te porous structure of te Biodentine surface, wic may ave eliated te difference between SE and ER tecniques. In addition, Biodentine wic as alkaline propertiesmay reduce te effect of bonding tecniques by buffering teir acidity [25]. In te present study, te most of te specimens exibited coesive failure in Biodentine. Te least common of te observed types of failure was adesive. Tis result reflects te inner coesion power of te coesive rater tan te real interfacial bond strengt of te adesive resin and te material. Coesive failures in restorative material or dentin may be due to te low internal resistance of te material or te bond strengt being greater tan te material s internal resistance [31]. In SEM and stereomicroscope images, wile more superficial coesive failures are observed witin Biodentine in groups [Figure 2A], deeper coesive failures were seen in groups [Figure 2B]. It may be suggested tat te superficial failure in groups may result from polymerization srinkage of te compomer placed on Biodentine. Te curing contraction of te compomer may lead to stresses, resulting in premature failures in weak Biodentine wic is in early sensitive pase. Tis finding sould be addressed carefully, as it may affect decisions to immediately place te restoration on Biodentine [25]. In conclusion, based on te data of tis study, it may Bond strengt, Biodentine universal adesive be concluded tat before applying compomer material on Biodentine, a waiting period of at least can be useful to obtain ig SBS values. It may be suggested tat sufficient bonding performance may also be obtained witout an acid etcing procedure, as universal adesive systems applied on Biodentine sow similar bond values in SE and ER modes. In tis way, ease of use is provided for particularly uncooperative pediatric patients by te reduced number of procedure steps, and te risk of contaation wit saliva is also reduced. DECLARATIONS Acknowledgments We tank Dr. Jon Wagner for is contribution in language editing. Autors contributions Manuscript s preparation: S. Aksoy Manuscript s review: M. Ünal Financial support and sponsorsip Tis study is supported by CÜBAP (DİŞ-142). Conflicts of interest Te autors deny any conflicts of interest related to tis study. Patient consent Not applicable. Etics approval Tis study as started to work after te approval of etics committee, Faculty of Medicine, Cumuriyet University Faculty of Medicine Clinical Researc and Etics Committee ( /16). REFERENCES 1. Asgary S, Egbal MJ. Treatment outcomes of pulpotomy in permanent molars wit irreversible pulpitis using biomaterials: a multi-center randomized controlled trial. Acta Odontol Scand 2013;71: Egbal MJ, Asgary S, Baglue RA, Parirok M, Goddusi J. MTA pulpotomy of uman permanent molars wit irreversible pulpitis. Aust Endod J 2009;35: Antunes Bortoluzzi E, Juárez Broon N, Antonio Hungaro Duarte M, de Oliveira Demarci AC, Monteiro Bramante C. Te use of a setting accelerator and its effect on ph and calcium ion release of eral trioxide aggregate and wite Portland cement. J Endod 2006;32: Camilleri J. Investigation of Biodentine as dentine replacement material. J Dent 2013;41: Bortoluzzi EA, Broon NJ, Bramante CM, Felippe WT, Tanomaru Filo M, Esberard RM. Te influence of calcium cloride on te setting time, solubility, disintegration, and ph of eral trioxide aggregate and wite Portland cement wit a radiopacifier. J Endod 2009;35: Grec L, Mallia B, Camilleri J. Investigation of te pysical properties of tricalcium silicate cement-based root-end filling materials. Dent 1

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