Use of nanoparticulate zinc oxide as intracanal medication in endodontics: pH and antimicrobial activity.

The aim of this study was to evaluate the pH and antimicrobial activity of micro or nanoparticulate zinc oxide (ZnO) pastes with or without calcium hydroxide (CH). The following medications were evaluated: microparticulate ZnO + polyethylene glycol (PEG) 400; nanoparticulate ZnO + PEG 400; PEG 400; CH + microparticulate ZnO + PEG 400 and CH + nanoparticulate ZnO + PEG 400. The pH was assessed between 12 hours and 28 days, using a digital pH meter. The antimicrobial activity against Enterococcus faecalis (ATCC-9212), Candida albicans (ATCC-10231), Pseudomonas aeruginosa (ATCC-27853), Staphylococcus aureus (ATCC-6538) and Kocuria rhizophila (ATCC-9341) was determined in triplicate using agar diffusion test. The results were submitted to Kruskal-Wallis/Dunn and ANOVA/Tukey tests with 5% significance. The highest pH values were found for CH+ZnO, with higher values for nanoparticulate ZnO after 12 hours and 21 days (p < 0.05). CH+ZnO medication promoted higher growth inhibition against P. aeruginosa and lower against E. faecalis. Calcium hydroxide pastes have higher pH and antimicrobial activity when associated with either micro- or nanoparticulate zinc oxide.

Titanium dioxide and modified titanium dioxide by silver nanoparticles as an anti biofilm filler content for composite resins.

OBJECTIVE: The aim of this study was to evaluate the antibacterial activity of a composite resin modified by TiO2 and TiO2/Ag nanoparticles and their influence over different properties. METHODS: TiO2 and TiO2/Ag NPs were synthesized by polymeric precursor and microwave-assisted hydrothermal methods and then, characterized by different techniques. Direct contact test was performed using Filtek™ Z350XT blended with 0.5; 1 and 2% (wt.) of NPs against Streptococcus mutans to determine the best concentration to the other tests. After that, the modified composite resin was tested against S. mutans 7-day biofilm (CFU/mL). Also, compressive and diametral tensile strength (n=40), degree of conversion (n=25) and surface roughness (n=50) was performed. The data were analyzed by ANOVA and Tukey's test for multiple comparison at 5% significance level. RESULTS: The direct contact test demonstrates that by increasing the nanoparticle content, the bacterial growth is significantly reduceed (p<0.05). The inclusion of 2% of TiO2/Ag NPs significantly decreased (p<0.05) the biofilm accumulation of S. mutans on the composite resin surface compared to the control Group. The TiO2 NPs treated with an organosilane increased compressive strength of composite resin (p<0.05). Degree of conversion remained unchanged (p>0.05) and the surface roughness increased with the NPs (p<0.05), except for the TiO2 by polymeric precursor Group (p>0.05). SIGNIFICANCE: The development of an antibacterial dental restorative material that hinder S. mutans biofilm without sacrificing the mechanical and physical properties is desirable in dental material science.

Synthesis, characterization and application of Ag doped ZnO nanoparticles in a composite resin.

The biofilm accumulation over the composite resin restorations can contribute to the formation of secondary caries. In this way, antibacterial restorative composite resins are highly desired. Then, the purpose of this study was to modify a composite resins using Ag doped ZnO nanoparticles (NPs), evaluate the antibacterial and mechanical properties of the modified composite resin. The ZnO/AgNPs were synthesized by two different routes, polymeric precursor and coprecipitation methods, and characterized by thermal decomposition, X-ray diffraction, specific surface area by N2 desorption/desorption and scanning electron microscopy (SEM). Antibacterial activity of composite resin specimens (4 mm in height and 2 mm in diameter; n = 15) modified by ZnO/Ag nanoparticles was performed against 7-days Streptococcus mutans biofilm. Colony forming units (CFU/mL) were used to evaluate the bacterial activity. Additionally, the morphology and the bacteria adherence area were analyzed by SEM images. Cylindrical specimens (6 mm in height and 4 mm in diameter; n = 20) of the composite resin containing ZnO/Ag NPs were prepared to perform compressive strength in a universal mechanical test machine, and the surface of fractured specimens was analyzed by EDX element mapping to verify NPs homogeneity. The normal distribution was confirmed and the two-way analysis of variance (ANOVA) and Tukey's test for pair comparison were performed. The nanospheres of ZnO/Ag lead to a better biofilm inhibition, than nanoplates. No difference on compressive strength was found for the composite resin modified by ZnO/Ag nanoplates. Based on these results, this material could be a good option as a new restorative material.

Zinc oxide 3D microstructures as an antimicrobial filler content for composite resins.

The aim of this study was to evaluate the antibacterial activity of a composite resin modified by 3D zinc oxide (ZnO) microstructures and to verify possible alterations on its mechanical properties. ZnO was synthesized by hydrothermal approach and characterized by X-ray diffraction (XRD), surface area by Brunauer, Emmett and Teller (BET), Fourier transform infrared spectroscopy (FTIR) and Field emission scanning electron microscopy (FESEM). The minimum inhibitory concentrations of ZnO against Streptococcus mutans, Escherichia coli, Staphylococcus aureus, and Candida albicans were determinated. The composite resin FiltekTM Z350XT (3M of Brazil) was blended with 0.2%, 0.5%, and 1% in weight of ZnO and submitted to antibacterial assay by direct contact test against S. mutans, the leading cause of dental caries and the most cariogenic oral streptococci. Additionally, it was performed compressive and diametral tensile strength tests of the modified composite resin. Microrods and hollow microrods of ZnO were obtained and its MIC values were found to be 125 µg/mL for S. mutans, 500 µg/mL for C. albicans and 62.5 µg/mL for S. aureus. For the tested concentrations, it was not found MIC against E. coli. The direct contact test showed a significant antibacterial capacity of modified composite resin (p > 0.05 for all concentrations). The compressive and diametral tensile strength remains no changed after inclusion of microparticles (p > 0.05 for all concentrations). The modification of the composite resin with small amounts of ZnO microparticles significantly inhibited the S. mutans growth on resin surface without significant alterations of its mechanical strength.

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.

Radiopacity and cytotoxicity of Portland cement associated with niobium oxide micro and nanoparticles.

OBJECTIVE: Mineral Trioxide Aggregate (MTA) is composed of Portland Cement (PC) and bismuth oxide (BO). Replacing BO for niobium oxide (NbO) microparticles (Nbµ) or nanoparticles (Nbη) may improve radiopacity and bioactivity. The aim of this study was to evaluate the radiopacity and cytotoxicity of the materials: (1) PC; (2) White MTA; (3) PC+30% Nbµ; (4) PC+30% Nbη. MATERIAL AND METHODS: For the radiopacity test, specimens of the different materials were radiographed along an aluminum step-wedge. For cell culture assays, Saos-2 osteoblastic-cells (ATCC HTB-85) were used. Cell viability was evaluated through MTT assay, and bioactivity was assessed by alkaline phosphatase activity assay. RESULTS: The results demonstrated higher radiopacity for MTA, followed by Nbµ and Nbη, which had similar values. Cell culture analysis showed that PC and PC+NbO associations promoted greater cell viability than MTA. CONCLUSIONS: It was concluded that the combination of PC+NbO is a potential alternative for composition of MTA.

Radiopacity, pH and antimicrobial activity of Portland cement associated with micro- and nanoparticles of zirconium oxide and niobium oxide.

The aim of this study was to evaluate some properties of the calcium silicate materials Mineral Trioxide Aggregate (MTA) and Portland cement (PC) with microparticulated (micro) and nanoparticulated (nano) zirconium oxide (ZrO2) or niobium oxide (Nb2O5). The experimental materials: White PC (PC), MTA-Angelus(®) (MTA), PC+ZrO2micro, PC+ZrO2nano, PC+Nb2O5micro and PC+Nb2O5nano were submitted to radiopacity and pH evaluations. Furthermore, the antimicrobial activity against different microorganisms was assessed by agar diffusion test. MTA presented higher radiopacity than other materials. However, all materials except PC presented higher radiopacity than recommended by ISO/ADA. MTA promoted higher pH values in all analyzed periods (p≤0.05). At the initial periods, PC and PC+ZrO2micro showed pH similar to MTA. All materials showed antimicrobial activity against the evaluated microorganisms. In conclusion, ZrO2 and Nb2O5 could be alternative radiopacifiers to be added to calcium silicate materials.

Antibacterial activity of intracanal medications based on calcium hydroxide and zinc oxide micro- or nanoparticles: an ex vivo study / Atividade antibacteriana de medicações intracanal à base de hidróxido de cálcio e óxido de zinco micro- e nanoparticulado: estudo ex vivo

Introduction: Nanoparticles and associations to calcium hydroxide can be used to increase antimicrobial activity. Objective: To evaluate antibacterial activity against Enterococcus faecalis and pH of intracanal medications (IM) based on calcium hydroxide (CH) and zinc oxide (ZnO) micro- or nanoparticles, and their association with 0.4% chlorhexidine (CHX). Material and method: Root canals from single-rooted human teeth were inoculated and incubated for 21 days. After sample (S1), the root canals were filled with the medications for 7 days and samples were collected immediately after medication (S2) and 7 days later (S3). Counting of CFU mL-1 was performed. Polyethylene tubes filled with the medications were used for the pH evaluation after 3, 7, 14 and 28 days. Data were submitted to ANOVA and Tukey tests (p<0.05). Result: All IM promoted elimination of E. faecalis immediately after medication (S2). All the pastes promoted a similar pH increase. Conclusion: CH/ZnO micro- or nanoparticles associated with CHX promoted greater bacterial reduction in the root canals and similar pH.

Introdução: Nanopartículas e associações ao hidróxido de cálcio podem ser usados para aumentar a ação antimicrobiana. Objetivo: Avaliar a atividade antibacteriana sobre Enterococcus faecalis e o pH de medicações intracanal (MI) à base de hidróxido de cálcio (HC) e óxido de zinco (OZn) micro- e nanoparticulado, e suas associações com clorexidina (CHX) a 0,4%. Material e método: Canais radiculares de dentes humanos unirradiculados foram inoculados e incubados por 21 dias. Após coleta (C1), os canais radiculares foram preenchidos com os medicamentos durante 7 dias e as amostras foram coletadas imediatamente após a medicação (C2) e 7 dias depois (C3). Contagem de UFC mL-1 foi realizada. Os tubos de polietileno preenchidos com os medicamentos foram utilizados para a avaliação do pH após 3, 7, 14 e 28 dias. Os dados foram submetidos aos testes de ANOVA e Tukey (p<0,05). Resultado: Todas as MI promoveram eliminação de E. faecalis imediatamente após a medicação (C2). Todas as pastas promoveram similar aumento de pH. Conclusão: HC/OZn micro- ou nanoparticulado associado com CHX promove maior redução bacteriana nos canais radiculares e pH similar.

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.

Radiopacity and cytotoxicity of Portland cement associated with niobium oxide micro and nanoparticles

Objective Mineral Trioxide Aggregate (MTA) is composed of Portland Cement (PC) and bismuth oxide (BO). Replacing BO for niobium oxide (NbO) microparticles (Nbµ) or nanoparticles (Nbη) may improve radiopacity and bioactivity. The aim of this study was to evaluate the radiopacity and cytotoxicity of the materials: 1) PC; 2) White MTA; 3) PC+30% Nbµ; 4) PC+30% Nbη. Material and Methods For the radiopacity test, specimens of the different materials were radiographed along an aluminum step-wedge. For cell culture assays, Saos-2 osteoblastic-cells (ATCC HTB-85) were used. Cell viability was evaluated through MTT assay, and bioactivity was assessed by alkaline phosphatase activity assay. Results The results demonstrated higher radiopacity for MTA, followed by Nbµ and Nbη, which had similar values. Cell culture analysis showed that PC and PC+NbO associations promoted greater cell viability than MTA. Conclusions It was concluded that the combination of PC+NbO is a potential alternative for composition of MTA. .