Self-etching dentine bonding agents are a recent addition to the choice of bonding agents which a clinician has available to bond resin restorations to tooth structure. The so-called ‘traditional’, total-etch fourth and fifth generation dentine bonding agents have proven their clinical abilities and the question now remains whether these ‘new’ self-etching dentine bonding agents will clinically perform as well as the ‘proven’ total-etch dentine bonding agents. For the purpose of this dissertation the author completed three research projects which were performed to evaluate the efficacy of a selection of dentine bonding agents and then used the results to compare some properties (shear bond strength, microleakage, and anti-bacterial properties) of total-etch dentine bonding agents with some self-etching dentine bonding agents. All discussions will focus on the three dentine bonding agent properties evaluated by the three research projects performed. The three specific aims of this study were: <ul> <li> To compare the dentine shear bond strength of a selection of self-etching dentine bonding agents with that of a total-etch dentine bonding agent control.</li> <li> To compare dentine and enamel microleakage values of a selection of self-etching bonding agents with that of a total-etch dentine bonding agent control.</li> <li> To evaluate the possible anti-bacterial properties of a selection of dentine bonding agents, with focus placed on the self-etching dentine bonding agent ABFb (Clearfil Protect Bond).</li></ul> The studies performed by the author achieved comparative/similar results to some studies described in the literature but it is clear from the literature that some studies provide conflicting results, especially leakage of enamel margins when using self-etching bonding agents. Taking into consideration the limitations of the three studies performed, it can be concluded that as far as the three evaluated properties of self-etching dentine bonding agents are concerned, they should prove to be acceptable clinical alternatives for use in place of total-etch dentine bonding agents. Copyright / Dissertation (MSc(Odont))--University of Pretoria, 2010. / Odontology / unrestricted

Philosophiae Doctor - PhD / Introduction: Biocompatibility of all kinds of dental materials is of paramount importance In order to prevent/limit irritation or degeneration of the surrounding tissues where it is applied. Some researchers suggested that dentine bonding agents may be used for pulpal protection, while pulpal inflammation and inhibition of pulpal repair following the use of dentine bonding agents were also reported. Objectives: The first part of this study compared the cytotoxicity of human pulp cell lines to a mouse 3T3 cell line to cytotoxic challenges from dentine bonding agents. The second part of the study compared the cytotoxicity of recent dentine bonding agents namely, Scotchbond 1, Prime & Bond NTand Xeno III through artificial membranes as well as thin dentine discs (after its reaction with apatite) and Clearfil Protect Bond (CPB)as such, as well as the primer part of CPBand the bond part of CPB separately. Methods and Materials: Near confluent human pulp cells and 3T3 cells were exposed to culture medium (DMEM)extractions from the various polymerized agents mentioned above and the cell viability (survival rate) was measured using the standard MTTassay and related to the non-exposed controls. Results: Two human pulp cells lines were more sensitive to 3T3 cell lines while the other human cell line was less sensitive to the 3T3 cell line. All bonding agents as such were found to be cytotoxic towards the 3T3 cells with Xeno III (25%survival rate) and CPB (35%)the most cytotoxic. Of the two parts from CPB the bond part was the least toxic (91% survival rate), but the primer part (containing the anti-bacterial pyridinium molecule) was very toxic (30% survival rate). ScotchBond 1 (59% survival rate) and Prime & Bond NT (62% survival rate) were not statistically different (Kruskal-Wallis Test, p>0.05). However,the survival rate of Xeno III (25% through membrane as well as dentine discs) and Clearfil Protect Bond (35%) were significantly lower than that of the other two bonding agents, with Xeno III significantly the most toxic (p<0.05 ) Conclusion: In general, all 4 dentine bonding agents were cytotoxic of which Xeno III was the most toxic even after its reaction with apatite (through dentine discs). The most toxic part of CPB was found to be the primer part containing the pyridinium linked molecule. If human pulp fibroblasts are used for cytotoxicity testing of dentine bonding agents many cell lines must be used.

Resin based composite is currently one of the most popular dental restoratives. Used as a direct restorative material, it displays many beneficial properties such as excellent micromechanical bonding to enamel, polishability and aesthetics. Despite many advances in dentine bonding agents, dentine bonding remains problematic with microleakage and recurrent caries, being frequent clinical sequelae. The open sandwich technique was developed to overcome two problems: deficient bonding of resin composites to dentine, and inadequate strength and fracture toughness of conventional glass-ionomers (GI). GI displayed excellent cavity sealing abilities by virtue of their chemical adhesion to tooth structure. Resin-modified glass-ionomers (RMGI) were developed to improve on the weaknesses of conventional GI during early setting i.e. setting rate, water sensitivity and strength. Recently literature has reported the use of ultrasonic activation to set conventional GI, opening the possibility of improving the initial properties of the material and suitability for use in the open sandwich technique. The aim of this study was to compare microleakage of Ketac Molar, Ketac Molar set by ultrasound (US), Vitremer and Ketac N100 used in the open sandwich technique, with the control of a resin based composite, Filtek Z250. Two hundred Class II cavities were prepared in a hundred caries free, human, molar teeth, with half of the cervical margins placed apical and the rest coronal to the cemento-enamel junction. For each material, twenty restorations were placed for each cervical position. The sandwich materials were placed to fill the interproximal box level with the pulpal floor, and a final two layers of resin composite was then placed to complete the restoration. Restored teeth were stored in a laboratory oven for 7 days at 37 °C; margins were then finished initially with a medium grit Sof-Lex disc and finally with a fine diamond drill. Material groups were separated into two halfs to commence microleakage testing or thermocycling. Thermocycling was conducted for 500 cycles between 5 °C and 55 °C, with a dwell time of 30 seconds. Restored teeth were then covered with nail varnish around the restoration margins, and immersed in 0.5% basic fuchsin solution for 24 hours. They were then cleaned, embedded in clear self-curing acrylic and sectioned 3 times with an Accutom-2 precision saw, at 2 mm intervals. Sections were evaluated using a light microscope under 4 time’s magnification and microleakage scores given as: 0 = no leakage; 1 = < ½; 2 = > ½ distance to the axial wall/pulpal floor; 3 = leakage up to axial wall/pulpal floor. Statistical analysis was undertaken using Analysis of Variance (ANOVA) for the cervical and occlusal microleakage scores; p-values <0.05 were considered significant. The cervical microleakage results of cavity margins in dentine showed that Ketac Molar (US) performed better than Ketac Molar, and Ketac N100 performed better than Vitremer. Results in enamel showed no significant differences. The use of the open sandwich technique effectively reduced microleakage of cervical cavity margins placed in dentine but failed to reduce occlusal microleakage of Filtek Z250. Copyright / Dissertation (MSc(Odont))--University of Pretoria, 2008. / Odontology / unrestricted

O objetivo do presente estudo foi desenvolver e caracterizar resinas adesivas contendo hidroxietil acrilamida (HEAA). Três grupos de resinas adesivas foram formulados, GHEAA33% (33,3% de HEAA + 66,6% de bisfenol A glicedil dimetacrilato - BisGMA), GHEAA50% (50% de HEAA + 50% de BisGMA) e GHEMA (33,3% de hidroxietil metacrilato - HEMA + 66,6% de BisGMA). Parâmetros como resistência à flexão (n= 12), grau de inchamento (n= 3), temperatura de transição vítrea (n= 3) e degradação em solvente (n= 5) foram avaliados de cada resina adesiva. Em adição foi avaliado com calorimetria exploratória diferencial (DSC), o processo de polimerização das resinas experimentais (n= 3), bem como dos homopolímeros componentes, BisGMA, HEMA, HEAA, HEMA* sem adição de etil 4- dimetilaminobenzoato (EDAB) e HEAA* sem adição de EDAB. Os resultados foram analisados estatisticamente com auxílio de ANOVA de uma via, teste de Tukey e teste t pareado. Todas as resinas adesivas e homopolímeros, exceto HEMA, HEAA* e HEMA*, apresentaram uma alta taxa de polimerização e um alto grau de conversão. Não houve diferença estatística entre as resinas adesivas para a temperatura de transição vítrea e a degradação em solvente (p>0,05). Entretanto, o grupo GHEAA33% apresentou a menor variação de grau de inchamento (p<0,05) e os menores valores de resistência à flexão (p<0,05) quando comparado com o grupo GHEMA. Considerando que a hidroxietil acrilamida foi capaz de promover o aumento do processo de polimerização de resinas adesivas experimentais e, tendo em vista sua potencial resistência à degradação hidrolítica e ainda, com base nos resultados dos demais ensaios, o grupo GHEAA33%, parece reunir as melhores condições de desenvolvimento de resinas adesivas inovadoras. / The purpose of this study was to develop an experimental adhesive resin using hydroxyethyl acrylamide (HEAA). Three groups of experimental resin were formulated, GHEAA33% (33.3% HEAA + 66.6% Bisphenol A glycerolate dimethacrylate- BisGMA), GHEAA50% (50% HEAA + 50% BisGMA), and GHEMA (33.3% 2-Hydroxyethyl methacrylate- HEMA + 66.6% of BisGMA). Parameters such as flexural strength (n= 12), swelling degree (n= 3), glass transition temperature (n= 3), and softening in solvent (n= 5) were evaluated for each adhesive resin. In addition, the polymerization process of each adhesive resin group (n= 3), as well as for the homopolymers, BisGMA, HEMA, HEAA, HEMA* without ethyl 4-dimethylaminobenzoate (EDAB), and HEAA* without EDAB, were also evaluated using differential scanning calorimetry (DSC). The results were analyzed using one way ANOVA, Tukey’s test, and Student’s t-test. For all of the resins and homopolymers evaluated, except for homopolymers HEMA, HEMA* and HEAA* homopolymer, a high rate of polymerization and a high degree of conversion were observed. There was no significant difference (p > 0.05) for the glass transition temperature and for softening in solvent for the adhesive resins assayed. In contrast, the GHEAA33% group exhibited less swelling degree (p < 0.05) and reduced flexural strength (p < 0.05) compared to the GHEMA group. HEAA was also found to promote the polymerization process and was resistant to hydrolytic degradation. Thus, GHEAA33% appears to be a promising alternative for the production of innovative adhesive resins.

O objetivo do presente estudo foi desenvolver e caracterizar resinas adesivas contendo hidroxietil acrilamida (HEAA). Três grupos de resinas adesivas foram formulados, GHEAA33% (33,3% de HEAA + 66,6% de bisfenol A glicedil dimetacrilato - BisGMA), GHEAA50% (50% de HEAA + 50% de BisGMA) e GHEMA (33,3% de hidroxietil metacrilato - HEMA + 66,6% de BisGMA). Parâmetros como resistência à flexão (n= 12), grau de inchamento (n= 3), temperatura de transição vítrea (n= 3) e degradação em solvente (n= 5) foram avaliados de cada resina adesiva. Em adição foi avaliado com calorimetria exploratória diferencial (DSC), o processo de polimerização das resinas experimentais (n= 3), bem como dos homopolímeros componentes, BisGMA, HEMA, HEAA, HEMA* sem adição de etil 4- dimetilaminobenzoato (EDAB) e HEAA* sem adição de EDAB. Os resultados foram analisados estatisticamente com auxílio de ANOVA de uma via, teste de Tukey e teste t pareado. Todas as resinas adesivas e homopolímeros, exceto HEMA, HEAA* e HEMA*, apresentaram uma alta taxa de polimerização e um alto grau de conversão. Não houve diferença estatística entre as resinas adesivas para a temperatura de transição vítrea e a degradação em solvente (p>0,05). Entretanto, o grupo GHEAA33% apresentou a menor variação de grau de inchamento (p<0,05) e os menores valores de resistência à flexão (p<0,05) quando comparado com o grupo GHEMA. Considerando que a hidroxietil acrilamida foi capaz de promover o aumento do processo de polimerização de resinas adesivas experimentais e, tendo em vista sua potencial resistência à degradação hidrolítica e ainda, com base nos resultados dos demais ensaios, o grupo GHEAA33%, parece reunir as melhores condições de desenvolvimento de resinas adesivas inovadoras. / The purpose of this study was to develop an experimental adhesive resin using hydroxyethyl acrylamide (HEAA). Three groups of experimental resin were formulated, GHEAA33% (33.3% HEAA + 66.6% Bisphenol A glycerolate dimethacrylate- BisGMA), GHEAA50% (50% HEAA + 50% BisGMA), and GHEMA (33.3% 2-Hydroxyethyl methacrylate- HEMA + 66.6% of BisGMA). Parameters such as flexural strength (n= 12), swelling degree (n= 3), glass transition temperature (n= 3), and softening in solvent (n= 5) were evaluated for each adhesive resin. In addition, the polymerization process of each adhesive resin group (n= 3), as well as for the homopolymers, BisGMA, HEMA, HEAA, HEMA* without ethyl 4-dimethylaminobenzoate (EDAB), and HEAA* without EDAB, were also evaluated using differential scanning calorimetry (DSC). The results were analyzed using one way ANOVA, Tukey’s test, and Student’s t-test. For all of the resins and homopolymers evaluated, except for homopolymers HEMA, HEMA* and HEAA* homopolymer, a high rate of polymerization and a high degree of conversion were observed. There was no significant difference (p > 0.05) for the glass transition temperature and for softening in solvent for the adhesive resins assayed. In contrast, the GHEAA33% group exhibited less swelling degree (p < 0.05) and reduced flexural strength (p < 0.05) compared to the GHEMA group. HEAA was also found to promote the polymerization process and was resistant to hydrolytic degradation. Thus, GHEAA33% appears to be a promising alternative for the production of innovative adhesive resins.

O objetivo do presente estudo foi desenvolver e caracterizar resinas adesivas contendo hidroxietil acrilamida (HEAA). Três grupos de resinas adesivas foram formulados, GHEAA33% (33,3% de HEAA + 66,6% de bisfenol A glicedil dimetacrilato - BisGMA), GHEAA50% (50% de HEAA + 50% de BisGMA) e GHEMA (33,3% de hidroxietil metacrilato - HEMA + 66,6% de BisGMA). Parâmetros como resistência à flexão (n= 12), grau de inchamento (n= 3), temperatura de transição vítrea (n= 3) e degradação em solvente (n= 5) foram avaliados de cada resina adesiva. Em adição foi avaliado com calorimetria exploratória diferencial (DSC), o processo de polimerização das resinas experimentais (n= 3), bem como dos homopolímeros componentes, BisGMA, HEMA, HEAA, HEMA* sem adição de etil 4- dimetilaminobenzoato (EDAB) e HEAA* sem adição de EDAB. Os resultados foram analisados estatisticamente com auxílio de ANOVA de uma via, teste de Tukey e teste t pareado. Todas as resinas adesivas e homopolímeros, exceto HEMA, HEAA* e HEMA*, apresentaram uma alta taxa de polimerização e um alto grau de conversão. Não houve diferença estatística entre as resinas adesivas para a temperatura de transição vítrea e a degradação em solvente (p>0,05). Entretanto, o grupo GHEAA33% apresentou a menor variação de grau de inchamento (p<0,05) e os menores valores de resistência à flexão (p<0,05) quando comparado com o grupo GHEMA. Considerando que a hidroxietil acrilamida foi capaz de promover o aumento do processo de polimerização de resinas adesivas experimentais e, tendo em vista sua potencial resistência à degradação hidrolítica e ainda, com base nos resultados dos demais ensaios, o grupo GHEAA33%, parece reunir as melhores condições de desenvolvimento de resinas adesivas inovadoras. / The purpose of this study was to develop an experimental adhesive resin using hydroxyethyl acrylamide (HEAA). Three groups of experimental resin were formulated, GHEAA33% (33.3% HEAA + 66.6% Bisphenol A glycerolate dimethacrylate- BisGMA), GHEAA50% (50% HEAA + 50% BisGMA), and GHEMA (33.3% 2-Hydroxyethyl methacrylate- HEMA + 66.6% of BisGMA). Parameters such as flexural strength (n= 12), swelling degree (n= 3), glass transition temperature (n= 3), and softening in solvent (n= 5) were evaluated for each adhesive resin. In addition, the polymerization process of each adhesive resin group (n= 3), as well as for the homopolymers, BisGMA, HEMA, HEAA, HEMA* without ethyl 4-dimethylaminobenzoate (EDAB), and HEAA* without EDAB, were also evaluated using differential scanning calorimetry (DSC). The results were analyzed using one way ANOVA, Tukey’s test, and Student’s t-test. For all of the resins and homopolymers evaluated, except for homopolymers HEMA, HEMA* and HEAA* homopolymer, a high rate of polymerization and a high degree of conversion were observed. There was no significant difference (p > 0.05) for the glass transition temperature and for softening in solvent for the adhesive resins assayed. In contrast, the GHEAA33% group exhibited less swelling degree (p < 0.05) and reduced flexural strength (p < 0.05) compared to the GHEMA group. HEAA was also found to promote the polymerization process and was resistant to hydrolytic degradation. Thus, GHEAA33% appears to be a promising alternative for the production of innovative adhesive resins.

CoordenaÃÃo de AperfeiÃoamento de Pessoal de NÃvel Superior / Existe um consenso de que a instabilidade da interface de uniÃo resina-dentina està relacionada com a quantidade de monÃmeros hidrofÃlicos presentes no sistema adesivo. Dessa forma, interfaces adesivas mais duradouras seriam alcanÃadas com a utilizaÃÃo de sistemas adesivos mais hidrofÃbicos. Uma maneira de unir monÃmeros hidrÃfobos à dentina à atravÃs da saturaÃÃo da matriz dentinÃria desmineralizada por etanol ao invÃs de Ãgua (ethanol-wet bonding technique). O objetivo deste trabalho in vitro foi avaliar o efeito do protocolo de saturaÃÃo dentinÃria, utilizando alcoÃis, na estabilidade da interface de uniÃo produzida por sistemas adesivos convencionais de dois passos. Para isso, foram utilizados 20 terceiros molares humanos, que tiveram a dentina coronÃria exposta e foram distribuÃdos aleatoriamente em quatro grupos experimentais (n=5): Adper Single Bond 2 (SB) aplicado sobre dentina saturada com Ãgua ou etanol; e XP Bond (XP) aplicado sobre dentina saturada com Ãgua ou tert-butanol. O protocolo de saturaÃÃo da dentina foi realizado atravÃs da aplicaÃÃo de 2 &#956;l de etanol 100% ou tert-butanol 99,5% diretamente sobre a dentina por um perÃodo de 60 s. Um platà de resina composta foi confeccionado sobre superfÃcie dentinÃria apÃs a aplicaÃÃo do sistema adesivo e os espÃcimes foram cortados pela tÃcnica non-trimming de obtenÃÃo de palitos para o teste de microtraÃÃo. Os palitos de cada dente foram igualmente divididos em dois subgrupos: imediatamente testado ou envelhecido em soluÃÃo de NaOCl a 10% por 1 hora. Os espÃcimes foram tracionados atà a ruptura da uniÃo a uma velocidade de 1 mm/min e sua forÃa de uniÃo mensurada. Os palitos fraturados foram analisados e classificados de acordo com o modo de fratura em mista, adesiva, coesiva em dentina e coesiva em compÃsito, e os valores expressos em porcentagem. Os valores de resistÃncia de uniÃo foram estatisticamente analisados usando os testes ANOVA a trÃs critÃrios e Tukey (&#945;=0.05). Discos extras de dentina foram submetidos aos procedimentos adesivos de cada grupo testado e utilizados para investigar as caracterÃsticas morfolÃgicas da interface de uniÃo atravÃs de microscopia Ãptica apÃs imersÃo em soluÃÃo amonical de nitrato de prata. Os resultados do teste de microtraÃÃo mostraram que a imersÃo em soluÃÃo de NaOCl reduziu significativamente a forÃa de uniÃo em comparaÃÃo aos grupos controle (p<0.05) e aumentou a nanoinfiltraÃÃo das interfaces adesivas de todos os sistemas adesivos testados. A saturaÃÃo da dentina com etanol 100% reduziu os valores de resistÃncia adesiva para SB quando comparado ao grupo controle, e esta mesma tendÃncia foi observada na infiltraÃÃo de prata. O uso do tert-butanol 99,5% nÃo afetou os valores de resistÃncia adesiva para o XP, assim como a deposiÃÃo de nitrato de prata na interface adesiva. ConclusÃo: Os protocolos simplificados de saturaÃÃo da dentina com alcoÃis utilizados no presente estudo nÃo foram capazes de melhorar a estabilidade da interface de uniÃo para sistemas adesivos convencionais de dois passos. / There is a consensus that the resin-dentin bond instability is correlated with increased hydrophilic resin monomer content in dentin adhesive. Thus, more durable bonds could be created when more hydrophobic resins were used. One way to bond hydrophobic monomers to acid-etched dentin is saturating the demineralized dentin with ethanol instead of water (ethanol-wet bonding technique). The objective of this in vitro study was to evaluate the effect of âalcohol wet bondingâ technique on the stability of adhesive interface produced by two-step etch-and-rinse adhesives systems. For this, it was used 20 human third molars that had superficial dentin exposed and were randomly divided into four experimental groups (n=5): Adper Single Bond 2 (SB) bonded to acid-etched dentin saturated with water or ethanol; and XP Bond (XP) bonded acid-etched dentin saturated with water or 99.5% tert-butanol. The simplified dentin dehydration protocol was performed using 2 &#956;l 100% ethanol or 99.5% tert-butanol directly applied in dentin for 60 s. Composite build-ups were built on dentin surface and specimens were cut into non-trimming dentin-composite beams to microtensile testing. Beams from each tooth were divided equally in two subgroups: immediately tested and aged by immersion in 10% NaOCl solution for 1 h. Specimens were pulled until failure at crosshead speed of 1 mm/min and bond strength was calculated. Fractured sticks were analyzed and classified according to the failure mode as mixed, adhesive, cohesive in dentin and cohesive in composite; and expressed in percentage. Data from &#956;TBS test were statistically analyzed using three-way ANOVA and Tukey tests (&#945;=0.05). Additional dentin disks were bonded using the same groups tested and the morphological characteristics of adhesive interface were investigated by light microscopy after immersion in ammoniacal silver nitrate solution. &#956;TBS results showed that NaOCl solution reduced significantly bond strength comparing with the control groups (p<0.05) and increased the silver nitrate interfacial deposit for all adhesives tested. SB used in ethanol saturated-dentin showed significant lower bond strength values in comparison with SB control group, and this same tendency was observed in the silver nitrate deposition. The use of tert-butanol did not influence XP bond strengths values and silver nitrate deposits. Conclusion: The âalcohol wet bondingâ simplified technique used in the present study was not able to improve resin-dentin bond stability for simplified etch-and-rinse adhesive systems.