Phosphoric acid containing proanthocyanidin enhances bond stability of resin/dentin interface

Abstract Proanthocyanidin (PA) is a promising dentin biomodifier due to its ability to stabilize collagen fibrils against degradation by matrix metalloproteinases (MMPs); however, the most effective protocol to incorporate PA into bonding procedures is still unclear. This study evaluated the effect of dentin biomodification with a PA acid etchant on MMP activity, adhesive interface morphology and resin-dentin microtensile bond strength. Sound extracted human molars were flattened to expose dentin and acid-etched for 15 s according to the groups: EXP - experimental phosphoric acid; EXP+PA - experimental phosphoric acid 10% PA; TE - total-etching system; SE - self-etching system. Samples were restored with composite resin and stored in distilled water (37ºC). MMP activity and interface morphology were analyzed after 24 h by in situ zymography (n=6) and scanning electron microscopy (n=3), respectively. The resin-dentin microtensile bond strength (μTBS) was evaluated after 24 h and 6 months storage (n=6). Significantly higher MMP activity was detected in etched dentin compared with untreated dentin (p<0.05), but no difference among acid groups was found. Resin tags and microtags, indicative of proper adhesive system penetration in dentinal tubules and microtubules, were observed along the hybrid layer in all groups. There was no difference in μTBS between 24 h and 6 months for EXP+PA; moreover, it showed higher long-term μTBS compared with TE and EXP (p<0.05). The results suggest that 15 s of biomodification was not sufficient to significantly reduce MMP activity; nonetheless, EXP+PA was still able to improve resin-dentin bond stability compared with total- and self-etching commercial systems.

Resumo A proantocianidina (PA) é um biomodificador dentinário promissor devido a sua capacidade de estabilizar as fibrilas colágenas contra a degradação por metaloproteinases da matriz (MMPs); no entanto, o protocolo mais eficaz para a incorporação de PA em procedimentos adesivos ainda não está claro. Este estudo avaliou o efeito da biomodificação da dentina com um condicionador ácido contendo PA na atividade de MMPs, morfologia da interface adesiva e resistência à microtração resina-dentina. Molares humanos extraídos foram lixados para exposição da dentina e condicionados com ácido por 15 s de acordo com os grupos: EXP - ácido fosfórico experimental; EXP+PA - ácido fosfórico experimental com 10% PA; TE - sistema total-etch; SE - sistema self-etch. As amostras foram restauradas com resina composta e armazenadas em água destilada (37ºC). A atividade de MMP e morfologia da interface foram analisadas após 24 h por zimografia in situ (n=6) e microscopia eletrônica de varredura (n=3), respectivamente. A resistência à microtração resina-dentina (μTBS) foi avaliada após 24 horas e 6 meses de armazenamento (n=6). Atividade de MMP detectada na dentina condicionada foi significativamente maior em comparação com a dentina não tratada (p <0,05), mas não houve diferenças entre os diferentes ácidos. Tags e microtags de resina, indicativos de uma penetração adequada do sistema adesivo nos túbulos e microtúbulos dentinários, foram observadas ao longo da camada híbrida em todos os grupos. Não houve diferença entre os valores de μTBS de 24 h e 6 meses para EXP+PA; além disso, EXP+PA apresentou maiores valores de μTBS após 6 meses em comparação com TE e EXP (p <0,05). Os resultados sugerem que a biomodificação por 15 s não foi suficiente para reduzir significativamente a atividade de MMP; apesar disso, EXP + PA foi capaz de melhorar a estabilidade da interface resina-dentina em comparação com sistemas total- e self-etch comerciais.

Avaliação do efeito de biopartícula nas propriedades mecânicas, químicas e estruturais longitudinais da interface adesiva em dentina: estudo "in vitro" / Evaluation of the bioparticle effect on the mechanical, chemical and longitudinal structural properties of the dentin adhesive interface: an "in vitro" study

Este estudo, desenvolvido em duas etapas, avaliou a ação remineralizadora da biopartícula α-wollastonita (BP), a partir da reação com H3PO4 residual Si-O-Ca + H3PO4 → SiO2 + Ca5(PO4)3(OH)n + H2O, na resistência longitudinal de união e características da interface adesiva, quando aplicada na forma de suspensão (etanol 99,5% + 10% de BP em peso) na superfície dentinária previamente condicionada com H3PO4 37%. Na primeira etapa foi realizado um estudo piloto onde, pelas características de precipitação, foi identificada a melhor concentração de biopartículas a serem inseridas na formulação da suspensão. Na segunda etapa, duzentas coroas hígidas de incisivos bovinos foram embutidas em resina acrílica, polidas para padronizar a smear layer e divididas aleatoriamente em 2 grupos (n=100), segundo a estratégia adesiva: A - controle (H3PO4 + Single Bond™ Universal (SB)); WAS ­ (H3PO4 + BP em suspensão + SB). Blocos de resina composta (Filtek Z250; 3M/ESPE) de 4mm foram confeccionados por técnica incremental sobre as áreas tratadas em todos os grupos, utilizando uma matriz de silicona. As amostras foram então seccionadas para obtenção de palitos retangulares (aproximadamente 1mm2 ), armazenadas em água deionizada a 4ºC em recipientes individuais e divididas em 2 subgrupos (n=50) de acordo com o tempo de armazenamento de 24 h (imediato) e 12 meses (longitudinal), seguidos do teste de resistência adesiva à microtração (10 kgf, 0,5mm/min). Os dados foram submetidos ao teste ANOVA 2 fatores (p< 0,05) e teste de Weibull 2 parâmetros. As interfaces adesivas foram analisadas por microscopia eletrônica de varredura (MEV) para avaliar a morfologia da interface resina-dentina, e analisadas por espectroscopia FTIR, para compreensão das interações químicas formadas na superfície dentinária. Os Resultados evidenciaram maiores valores estatisticamente significativos de resistência de união (MPa) para o grupo WAS (37,39 ± 7,48), tratado com BP e armazenado por 24 h, em comparação ao grupo A armazenado por 24 h (27,58 ± 6,43); e, para o grupo WAS armazenado por 12 meses (32,05 ± 10,64) em comparação ao grupo A armazenado por 12 meses (22,84 ± 5,76). Dados do FTIR evidenciaram o efeito da α-wollastonita na preservação do colágeno. A biopartícula mostrou ser promissora na manutenção longitudinal da qualidade da interface adesiva. (AU)

This study, developed in two stages, evaluated the remineralizing action of the αwollastonite (BP) bioparticle, from the reaction with residual Si-O-Ca + H3PO4 → SiO2 + Ca5(PO4)3(OH)n + H2O, on the longitudinal bond strength and characteristics of the adhesive interface, when applied as a suspension (99.5% ethanol + 10% BP by weight) on the dentin surface previously etched with 37% H3PO4. In the first stage, a pilot study was carried out where, due to the precipitation characteristics, the best concentration of bioparticles to be inserted in the suspension formulation was identified. In the second step, two hundred sound bovine incisor crowns were embedded in acrylic resin, polished to standardize the smear layer and randomly divided into 2 groups (n=100), according to the adhesive strategy: A - control (H3PO4 + Single Bond™ Universal (SB)); WAS ­ (H3PO4 + BP in suspension + SB). Composite resin blocks (Filtek Z250; 3M/ESPE) of 4 mm were made by incremental technique on the treated areas in all groups, using a silicone matrix. The samples were then sectioned to obtain rectangular sticks (approximately 1mm2 ), stored in deionized water at 4ºC in individual containers and divided into 2 subgroups (n=50) according to the storage time of 24 h (immediate) and 12 months (longitudinal), followed by the microtensile bond strength test (10 kgf, 0.5 mm/min). Data were submitted to 2-way ANOVA (p<0.05) and 2-parameter Weibull test. The adhesive interfaces were analyzed by scanning electron microscopy (SEM) to evaluate the morphology of the resin-dentin interface, and analyzed by FTIR spectroscopy, to understand the chemical interactions formed on the dentin surface. The results showed higher statistically significant values of bond strength (MPa) for the WAS group (37.39 ± 7.48), treated with BP and stored for 24 h, compared to group A stored for 24 h (27, 58 ± 6.43); and for the WAS group stored for 12 months (32.05 ± 10.64) compared to group A stored for 12 months (22.84 ± 5.76). FTIR data evidenced the effect of α-wollastonite on collagen preservation. The bioparticle showed promise in the longitudinal maintenance of the quality of the adhesive interface (AU)

The effect of adhesive with different unsealing time on the microleakage of adhesive interface / 实用口腔医学杂志

Objective: To investigate the effect of self-etching adhesive with different unsealing time on the microleakage of the adhesive interface between tooth and resin. Methods: Unopened self-etching adhesives, Scotchbond Universal (S) and Xeno V+ (X) were respectively used to adhere Z350 resin for restoration of the prepared occlusal cavities sized 4 mm × 4 mm × 4 mm (n = 40) . The methylene blue staining method was used to observe the microleakage of the adhesive interface between the tooth and filling material at the instant moment, 1, 2 and 3 months after the self-etching adhesives was opened (n = 10) . Results: (1) Increase of microleakage in S group was found with the time span after unsealing, and there was a statistical difference between the instant moment and 3 months after unsealing (P＜0. 05) . (2) There was no significant difference at the 4 test time points in X group (P＞0. 05), although the microleakage value of the samples were increased with the increase of the time after unsealing. (3) The microleakage of X group was greater than that of S group at the instant moment and 1 month after unsealing (P＜0. 05) . Conclusion: Unsealing time may increase the microleakage of the adhesive interface between the tooth and the filling material, the effect varies with the types of the adhesives.

Composite resins: a review of adhesive failure from enzymatic degradation

Aim: This study aims to review the concepts and metalloproteinase activation mechanisms and cathepsin cysteine. Material and Methods: The literature review was conducted around the main keywords "cathepsin cysteine", "metalloproteinases", "dentin-adhesive interface" and "degradation". Results: Nineteen articles were collected and included only articles available in its entirety, on english. Conclusions: Many studies are still being conducted incorporating different substances that help by inhibiting the action of these enzymes, however, there is still no consensus on the best element to be used in restorative procedures.

Influencia de los inhibidores de las metaloproteinasas, agentes reticuladores y remineralización biomimética en la longevidad de la unión adhesiva: parte 3: agentes reticuladores / Metalloproteinase inhibitors, cross-linking agents and biomimetic remineralization influence in the adhesive bond longevity: part 3: cross-linking agents

Las propiedades mecánicas del colágeno se deben a agentes intrínsecos de entrecruzamiento [Al-Ammar et al, 2009]. El aumento en el número de enlaces de la molécula de colágeno mejora su estabilidad e integridad, colaborando con el mantenimiento de propiedades adecuadas de la unión adhesiva a lo largo del tiempo [Bedran-Russo et al, 2009; Breschi et al, 2008]. Existen varios enfoques que permiten modificar el sustrato dentinario mediante la promoción de la formación de enlaces exógenos, con el objetivo de aumentar la resistencia de la red de colágeno [Bedran-Russo et al, 2007; Bedran-Russo et al, 2008]. Estos enfoques se dividen en métodos mecánicos [Bedran-Russo et al, 2007; Bedran-Russo et al, 2008; Castellan et al, 2010; Han et al, 2003] y método fotoxidativo [Cova et al, 2011]. Dentro de los primeros, los agentes reticuladores de origen natural son capaces de estabilizar el colágeno de la dentina [Bedran-Russo et al, 2007] sin afectar la resistencia de la unión adhesiva y sin generar toxicidad. Sin embargo, el uso de estos agentes por sí solo no permite asegurar la estabilidad de la unión adhesiva a lo largo del tiempo; porque como es sabido, la longevidad de dicha unión no depende únicamente de las características del sustrato, sino también de propiedades inherentes al sistema adhesivo por un lado, y de la presencia de humedad por otro.

The mechanical properties of collagen are due to intrinsic crosslinking agents [Al-Ammar et al, 2009]. The increase in the number of links of the collagen molecule improves its stability and integrity, collaborating with the maintenance of adequate adhesive bonding properties over time [Bedran-Russo et al, 2009; Breschi et al, 2008]. There are several approaches for modifying the dentin substrate by promoting the formation of exogenous links, in order to increase the strength of the collagen network [Bedran-Russo et al, 2007; Bedran-Russo et al, 2008]. These approaches are divided into mechanical methods [Bedran-Russo et al, 2007; Bedran-Russo et al, 2008; Castellan et al, 2010; Han et al, 2003] and foto oxidating method [Cova et al, 2011]. Within the first, the naturally occurring crosslinking agents are capable of stabilizing the dentin collagen [Bedran-Russo et al, 2007] without affecting the strength of the adhesive bond and without generating any toxicity. However, the use of these agents alone does not ensure the stability of the adhesive bond over time; because as it is known, the longevity of such binding does not only depend on the substrate’s characteristics, but also on the adhesive system’s properties on one side, and the presence of moisture on the other

Evaluación de la interfase adhesiva obtenida en restauraciones de resina compuesta realizadas con un sistema adhesivo universal utilizado con y sin grabado ácido previo / Evaluation of the adhesive interface obtained in composite restorations performed with a universal adhesive system used with and without acid etching

OBJETIVO El propósito de esta investigación fue realizar un estudio observacional in vitro, al microscopio electrónico de barrido, de la interfase adhesiva diente-restauración lograda al utilizar un sistema adhesivo universal (Single Bond Universal®, 3M/ESPE, Alemania), con grabado ácido previo y con la técnica de autograbado. MATERIALES Y MÉTODO En las piezas dentarias se realizaron cavidades clase V en las caras vestibular y palatina/lingual. En la cavidad vestibular se realizó la técnica de grabado ácido con H3PO4 al 37% en gel, mientras que en la cavidad palatina o lingual no se realizó grabado ácido. Las piezas restauradas fueron mantenidas en una estufa a 37 °C con 100% de humedad relativa durante 48 h, simulando el medio bucal. Las muestras obtenidas fueron cortadas a través de la restauración y acondicionadas para poder ser observadas al microscopio electrónico de barrido, para evaluar la interfase adhesiva en relación con la presencia de brechas y la formación de tags de resina. RESULTADOS Las imágenes fueron observadas con un aumento progresivo hasta los 2.000×, viéndose diferencias microestructurales en la penetración del adhesivo, aunque sin formación de brechas en la interfase adhesiva. CONCLUSIONES Se observó que, al utilizar ambas técnicas de aplicación se obtiene una interfase sin presencia de brechas. En esmalte, se generó una menor penetración del adhesivo en la estructura cristalina con la técnica de autograbado, mientras que en dentina, con la misma técnica, se genera una capa híbrida de menor espesor y tags de resina de menor longitud.

OBJECTIVE The purpose of this research was to study the tooth-restoration adhesive interface, using a universal adhesive system (Single Bond Universal, 3M/ESPE, Germany), with the techniques of etching and self-etching using scanning electron microscopy. MATERIALS AND METHODS Class V cavities were prepared in buccal and palatine/lingual surface, in human teeth. Etching with 37%H3PO4 was performed in the buccal cavity, with no etching being performed in the palatine or lingual cavity. The samples were placed in an oven at 37 °C and 100% humidity for 48 hours, simulating the oral environment. The samples were cut perpendicularly through the restoration and prepared to be observed by scanning electron microscopy, in order to evaluate the adhesive interface in relation to the presence of breaches and the formation of resin tags. RESULTS Images were observed with a gradual increase to 2000×. Microstructural differences were observed in the penetration of the adhesive but with no formation of breaches in the adhesive interface. CONCLUSIONS An unbreached interface is obtained when using both techniques. In enamel, less penetration was present in the crystal structure of the adhesive with the self-etching technique. While in dentin, with the same technique, a less thick hybrid layer and shorter resin tags were observed.

Elementos conceptuales para estudiar el comportamiento bioadhesivo en polímeros / Conceptual elements to study the bioadhesive behavior in polymers

La bioadhesión es un fenómeno interfacial que ocurre entre un material polimérico y una superficie biológica. Las interacciones entre las fases son el resultado tanto de las propiedades del polímero como de la naturaleza del sustrato. En este documento se estudian los aspectos teóricos fundamentales que permiten entender los mecanismos que se proponen para la interpretación del fenómeno desde cada una de las teorías existentes, considerando los factores que determinan el comportamiento bioadhesivo de un polímero y las características del sustrato. Finalmente se analizan las técnicas experimentales existentes para determinar la bioadhesividad en materiales poliméricos y las aplicaciones en el diseño de algunos sistemas terapéuticos farmacéuticos.

The bioadhesion is an interfacial phenomenon ocurring between a polymer and a biological surface. Due to the complex nature of polymers and molecules present in the biological surfaces, many factors determine the strength and duration of the adhesion. However, the specific interactions in the polymer/biological substrate interface are governed by both, the properties of the polymer and the nature of the substrate. In this document the theoretical fundamentals of the current mechanisms that have been proposed to explain bioadhesion are reviewed. Also, the main factors determining the bioadhesive behavior of a polymer and the properties of the substrate are discussed. Finally, the experimental techniques to evaluate the bioadhesion in polymers are analyzed, and the applications in some therapeutic pharmaceutical systems presented.