Effect of addition of nano-hydroxyapatite on physico-chemical and antibiofilm properties of calcium silicate cements.

OBJECTIVE: Mineral Trioxide Aggregate (MTA) is a calcium silicate cement composed of Portland cement (PC) and bismuth oxide. Hydroxyapatite has been incorporated to enhance mechanical and biological properties of dental materials. This study evaluated physicochemical and mechanical properties and antibiofilm activity of MTA and PC associated with zirconium oxide (ZrO2) and hydroxyapatite nanoparticles (HAn). MATERIAL AND METHODS: White MTA (Angelus, Brazil); PC (70%)+ZrO2 (30%); PC (60%)+ZrO2 (30%)+HAn (10%); PC (50%)+ZrO2 (30%)+HAn (20%) were evaluated. The pH was assessed by a digital pH-meter and solubility by mass loss. Setting time was evaluated by using Gilmore needles. Compressive strength was analyzed by mechanical test. Samples were radiographed alongside an aluminum step wedge to evaluate radiopacity. For the antibiofilm evaluation, materials were placed in direct contact with E. faecalis biofilm induced on dentine blocks. The number of colony-forming units (CFU mL-1) in the remaining biolfilm was evaluated. The results were submitted to ANOVA and the Tukey test, with 5% significance. RESULTS: There was no difference in pH levels of PC+ZrO2, PC+ZrO2+HAn (10%) and PC+ZrO2+HAn (20%) (p>0.05) and these cements presented higher pH levels than MTA (p<0.05). The highest solubility was observed in PC+ZrO2+HAn (10%) and PC+ZrO2+HAn (20%) (p<0.05). MTA had the shortest initial setting time (p<0.05). All the materials showed radiopacity higher than 3 mmAl. PC+ZrO2 and MTA had the highest compressive strength (p<0.05). Materials did not completely neutralize the bacterial biofilm, but the association with HAn provided greater bacterial reduction than MTA and PC+ZrO2 (p<0.05) after the post-manipulation period of 2 days. CONCLUSIONS: The addition of HAn to PC associated with ZrO2 harmed the compressive strength and solubility. On the other hand, HAn did not change the pH and the initial setting time, but improved the radiopacity (HAn 10%), the final setting time and the E. faecalis antibiofilm activity of the cement.

Effect of addition of nano-hydroxyapatite on physico-chemical and antibiofilm properties of calcium silicate cements

ABSTRACT Objective Mineral Trioxide Aggregate (MTA) is a calcium silicate cement composed of Portland cement (PC) and bismuth oxide. Hydroxyapatite has been incorporated to enhance mechanical and biological properties of dental materials. This study evaluated physicochemical and mechanical properties and antibiofilm activity of MTA and PC associated with zirconium oxide (ZrO2) and hydroxyapatite nanoparticles (HAn). Material and Methods White MTA (Angelus, Brazil); PC (70%)+ZrO2 (30%); PC (60%)+ZrO2 (30%)+HAn (10%); PC (50%)+ZrO2 (30%)+HAn (20%) were evaluated. The pH was assessed by a digital pH-meter and solubility by mass loss. Setting time was evaluated by using Gilmore needles. Compressive strength was analyzed by mechanical test. Samples were radiographed alongside an aluminum step wedge to evaluate radiopacity. For the antibiofilm evaluation, materials were placed in direct contact with E. faecalis biofilm induced on dentine blocks. The number of colony-forming units (CFU mL-1) in the remaining biolfilm was evaluated. The results were submitted to ANOVA and the Tukey test, with 5% significance. Results There was no difference in pH levels of PC+ZrO2, PC+ZrO2+HAn (10%) and PC+ZrO2+HAn (20%) (p>0.05) and these cements presented higher pH levels than MTA (p<0.05). The highest solubility was observed in PC+ZrO2+HAn (10%) and PC+ZrO2+HAn (20%) (p<0.05). MTA had the shortest initial setting time (p<0.05). All the materials showed radiopacity higher than 3 mmAl. PC+ZrO2 and MTA had the highest compressive strength (p<0.05). Materials did not completely neutralize the bacterial biofilm, but the association with HAn provided greater bacterial reduction than MTA and PC+ZrO2 (p<0.05) after the post-manipulation period of 2 days. Conclusions The addition of HAn to PC associated with ZrO2 harmed the compressive strength and solubility. On the other hand, HAn did not change the pH and the initial setting time, but improved the radiopacity (HAn 10%), the final setting time and the E. faecalis antibiofilm activity of the cement.

Evaluation of the interaction between sodium hypochlorite and several formulations containing chlorhexidine and its effect on the radicular dentin--SEM and push-out bond strength analysis.

The aim of the current study was to evaluate the presence of debris and smear layer after endodontic irrigation with different formulations of 2% chlorhexidine gluconate (CHX) and its effects on the push-out bond strength of an epoxy-based sealer on the radicular dentin. One hundred extracted human canines were prepared to F5 instrument and irrigated with 2.5% sodium hypochlorite and 17% ethylenediaminetetraacetic acid. Fifty teeth were divided into five groups (n = 10), according to the final irrigation protocol with different 2% CHX formulations: G1 (control, no final rinse irrigation), G2 (CHX solution), G3 (CHX gel), G4 (Concepsis), and G5 (CHX Plus). In sequence, the specimens were submitted to scanning electron microscopy (SEM) analysis, in the cervical-medium and medium-apical segments, to evaluate the presence of debris and smear layer. The other 50 teeth were treated equally to a SEM study, but with the root canals filled with an epoxy-based endodontic sealer and submitted to a push-out bond strength test, in the cervical, middle, and apical thirds. G2, G3, G4, and G5 provided higher precipitation of the debris and smear layer than G1 (P < 0.05), but these groups were similar to each other (P > 0.05), in both segments. The values obtained in the push out test did not differ between groups, independent of the radicular third (P > 0.05). The CHXs formulations caused precipitation of the debris and smear layer on the radicular dentin, but these residues did not interfere in the push-out bond strength of the epoxy-based sealer.

Avaliação de propriedades físico-químicas, mecânicas e antimicrobianos do MTA e cimento Portland associado a solução de nanopartículas de prata / Evaluation of physico-chemical, mechanical and antimicrobial properties of MTA and Portland cement associated with silver nanoparticles solution

A substituição do óxido de bismuto por óxido de zircônio (ZrO2) e a adição de nanopartículas de prata (NPsAg) pode favorecer as propriedades físico-químicas mecânicas e antimicrobianas. Capítulo 1: Foram avaliados pH, solubilidade, tempo de presa, radiopacidade e resistência à compressão. Grupos: G1 - MTA Angelus; G2 - CP/ZrO2; G3 - MTA/NPsAg; G4 -CP/ZrO2/NPsAg. O pH foi analisado em pHmetro digital, a solubilidade pela perda de massa e o tempo de presa pelo teste de Gilmore. A resistência à compressão foi avaliada em ensaio mecânico. Para análise da radiopacidade, as amostras foram radiografadas com uma escala de alumínio. Os resultados foram submetidos aos testes ANOVA e Tukey (p<0,05). O G3 apresentou aumento de pH e diminuição da solubilidade e tempo do presa inicial e final. O G4 apresentou diminuição da solubilidade e aumento da resistência à compressão. A radiopacidade dos materiais foi superior a 4 mmAl. As associações G3 e G4 apresentam propriedades físico-químicas e mecânicas adequadas. Capítulo 2: Bactérias na forma planctônica foram colocadas sobre o cimento fresco e a análise foi realizada em espectrofotômetro. Na avaliação antibiofilme, os materiais foram colocados em contato com biofilme de E. faecalis formado sobre blocos de dentina e analisados pela contagem de unidades formadoras de colônia. Os resultados foram submetidos aos testes ANOVA e Tukey (p<0,05). Na forma planctônica, melhores resultados foram encontrados no G2 e G4. Maior redução de biofilme foi apresentada pelos G3 e G4. A incorporação de NPsAg ao CP e MTA, melhora a atividade antibacteriana e antibiofilme dos materiais à base de silicato de cálcio.

The bismuth oxide replacement by zirconium oxide (ZrO2) and the addition of silver nanoparticles may improve the physicochemical, mechanic and antimicrobial properties. Chapter I: It was evaluated pH, solubility, setting time, radiopacity and compressive strength. Groups: G1-MTA Angelus; G2-PC/ZrO2; G3-MTA/NPsAg, G4-PC/ZrO2/NPsAg. The pH was measured with a digital pH meter, the solubility by the weight loss and the setting time was evaluated by Gilmore needle. Compressive strength was tested in universal testing machine. For radiopacity analysis material samples were radiographed alongside an aluminium step-wedge. The results were submitted to ANOVA and Tukey tests (p<0.05). The G3 showed a pH increase and a decrease of solubility and initial and final setting time. The G4 showed a decrease in solubility and an increase of compressive strength. All materials presented radiopacity greater than 4 mmAl. The G3 and G4 associations showed good physicochemical and mechanical properties. Chapter 2: For the first test bacterias in planktonic form were placed over fresh cement, and the analysis was performed in spectrophotometer. Also for the antibiofilm test, the samples were placed in direct contact with E. faecalis biofilm previously induced on bovine dentine and analysed by the counting of colony-forming units. The results were submitted to ANOVA and Tukey tests (p<0.05). On the planktonic form, the best results were showed by G2 and G4. The greater reduction of biofilm were showed by G3 and G4. The incorporation of NPsAg to PC and MTA improves the antibacterial and antbiofilm activity of calcium silicate cements

Actividad antimicrobiana de la solución de nanopartícula de plata en cultivo de Enterococcus faecalis / Antimicrobial activity of silver nanoparticles solution on culture of Enterococcus faecalis

Objetivo. El objetivo del estudio fue evaluar la actividad antimicrobiana de la solución de nanopartículas de plata en cultivo de Enterococcus faecalis (ATCC 29212) comparándola con diversas soluciones de hipoclorito de sodio (NaOCl). Material y Métodos. Cinco placas de Petri en agar fueron inoculadas con E. faecalis y sobre cada una de ellas se colocó un disco de celulosa saturado de solución de nanopartículas de plata, así como en cada una de las soluciones de hipoclorito de sodio evaluadas (Viarzon, Cloralex, Clorox). El digluconato de clorhexidina al 2% y solución salina estéril fueron utilizados como control. Transcurridas 24 horas de incubación a 37°C, en condiciones de aerobiosis, las zonas de inhibición de crecimiento bacteriano fueron medidas y los resultados sometidos a la prueba “t” entre los grupos experimentales (= 5%). Resultados. El Cloralex presentó la mayor media de inhibición en comparación con las demás substancias (p < 0,05), excepto con digluconato de clorhexidina al 2% (p > 0,05). La solución de nanopartículas de plata proporcionó mayor zona de inhibición que Clorox y Viarzon (p <0,05). El Clorox y el Viarzon no proporcionaron zonas de inhibición y fueron semejantes entre sí (p > 0,05). Conclusiones. La solución de nanopartículas de plata presenta actividad antimicrobiana en cultivo de E. faecalis, incluso mayor que las formas comerciales de hipoclorito de sodio. Futuros estudios deben ser realizados para comprobar su viabilidad como solución de irrigación en endodoncia (AU)

Objective. The objective of this study was to evaluate the antimicrobial activity of the silver nanoparticles solution in enterococcus faecallis cultures (ATCC 29212), compared with various solutions of sodium hypoclorithe (NaOCl). Material and methods. Five Agar Petri plates were inoculated with E. faecallis and each of them was placed a cellulose dish embedded with silver nanoparticles solution, or a solution of sodium hypochlorite evaluated (Viarzon, Cloralex, Clorox). Chlorhexidine digluconate 2% was used as positive control and sterile saline solution was used as negative control. After 24 hours of incubation at 37ºc, under aerobic conditions, the zones of inhibition of bacterial growth were measured and the results subjected to the statistical t test among the experimental groups (= 5%). Results. The Cloralex showed to be the most effective reflected in the extent of inhibition in relation to other substances (p< 0.05), except that the chlorhexidine digluconate 2% (p> 0.05). The solution of silver nanoparticles provided a greater zone of inhibition than the sodium hypochlorite solution (Clorox) and Viarzon (p< 0.05). Clorox and Viarzon didn’t provide zones of inhibition and were similar to each other (p> 0.05). Conclusions. The solution of silver nanoparticles presents antimicrobial activity in cultured E. faecallis, even higher than other commercial forms of sodium hypochlorite. Further studies should be carried out to determine its viability as irrigating solution in endodontics (AU)