Department of Restorative Dentistry, University of Campinas - Piracicaba Dental School, Piracicaba, SP, Brazil.
Department of Biosciences, University of Campinas, Piracicaba Dental School, Piracicaba, SP, Brazil.
J Mech Behav Biomed Mater. 2023 Jul;143:105919. doi: 10.1016/j.jmbbm.2023.105919. Epub 2023 May 25.
This study developed an experimental flowable composite incorporated with niobium pentoxide (NbO) combined or not with titanium dioxide co-doped with fluorine and nitrogen (NF_TiO) and evaluated the mechanical and antibacterial properties. The experimental flowable composite (TEGDMA + BisGMA 1:1 + 60%wt - inorganic filler - borosilicate 0.7 μm) was formulated according to the type and concentration of NbO and NF_TiO (0.5, 1, 1.5 and 2 wt%) or NF_TiO + NbO (0.25, 0.5, 0.75 and 1 wt% - 1:1). The control groups were formed by the experimental composite without the incorporation of NbO and/or NF_TiO (GC-E) and by a commercial flowable composite (GC). The characterization of the surface of the composite and its particles was carried out using scanning electron microscopy (SEM) and energy dispersive x-rays (EDX). Specimens were manufactured and subjected to mechanical tests of flexural strength (FS) (n = 12), flexural modulus (FM) (n = 12), roughness (Ra) (n = 10), microhardness (n = 10), and contact angle (n = 10); and, to evaluate the antibacterial activity, they were submitted to tests of biofilm formation against S. mutans (CFU/mL) (n = 5), biofilm biomass by dry weight (n = 5) and confocal laser microscopy (%LIVE/DEAD) (n = 5). Data were submitted to one-way ANOVA and Tukey's post-hoc and, those that were not homoscedastic, but with normality, were submitted to Welch's ANOVA and Games-Howell's post-hoc. Dunnet's test was used to compare the controls with the other experimental groups (α = 5). The NbO particles had an average size of 32.4 μm and the nanoparticles (NPs) of NF_TiO, 10 nm. EDX analysis identified isolated peaks of N, F, Ti, and Nb confirming the presence of these particles in the resin matrix. The 1.5% NF_TiO group had a higher FS and FM than the controls (p < 0.05). GC showed higher microhardness between groups (p < 0.05). There was no difference between the experimental groups regarding contact angle and roughness (p > 0.05), except for GC, which had the highest Ra values and the lowest contact angle between groups (p < 0.05). Composites containing 0.5%, 1%, 1.5%, and 2% NbO, 1%, 1.5%, and 2% NF_TiO and 2% NbO + NF_TiO showed lower biofilm formation (p < 0.05), lower total biofilm biomass (p < 0.05), and a higher percentage of dead cells (44%, 52%, 52%, 79%, 42% 43%, 62%, 65%, respectively) than GC and GC-E (5% and 1%, respectively). It is concluded that the incorporation of 1.5% NF_TiO promoted a greater FS and FM among the experimental composites and that the addition of NbO particles (0.5%, 1%, 1.5%, and 2%), NF_TiO (1%, 1.5% and 2%) and the combination NbO + NF_TiO (2%) showed significant antibacterial effects.
本研究开发了一种实验性可流动性复合材料,其中包含五氧化二铌(NbO),并结合或不结合掺氟和氮的二氧化钛(NF_TiO),并评估了其机械性能和抗菌性能。实验性可流动性复合材料(TEGDMA + BisGMA 1:1 + 60%wt-无机填料-硼硅酸盐 0.7μm)根据 NbO 和 NF_TiO(0.5、1、1.5 和 2wt%)或 NF_TiO + NbO(0.25、0.5、0.75 和 1wt%-1:1)的类型和浓度进行配方。对照组由不含 NbO 和/或 NF_TiO 的实验性复合材料(GC-E)和一种商业可流动性复合材料(GC)组成。使用扫描电子显微镜(SEM)和能量色散 X 射线(EDX)对复合材料及其颗粒的表面进行了表征。制造了样本,并进行了弯曲强度(FS)(n=12)、弯曲模量(FM)(n=12)、粗糙度(Ra)(n=10)、显微硬度(n=10)和接触角(n=10)的机械性能测试;为了评估抗菌活性,它们被用于测试对变形链球菌(CFU/mL)(n=5)的生物膜形成、干重的生物膜生物量(n=5)和共聚焦激光显微镜(%LIVE/DEAD)(n=5)。数据进行了单因素方差分析和 Tukey 的事后检验,对于那些非同方差但具有正态性的,则进行了 Welch 的方差分析和 Games-Howell 的事后检验。Dunnett 检验用于比较对照组和其他实验组(α=5)。NbO 颗粒的平均粒径为 32.4μm,NF_TiO 的纳米颗粒(NPs)为 10nm。EDX 分析鉴定出孤立的 N、F、Ti 和 Nb 峰,证实了这些颗粒存在于树脂基质中。1.5% NF_TiO 组的 FS 和 FM 高于对照组(p<0.05)。GC 显示出各组之间更高的显微硬度(p<0.05)。除 GC 外,各组之间的接触角和粗糙度无差异(p>0.05),GC 的 Ra 值最高,接触角最低(p<0.05)。含有 0.5%、1%、1.5%和 2% NbO、1%、1.5%和 2% NF_TiO 和 2% NbO + NF_TiO 的复合材料显示出较低的生物膜形成(p<0.05)、较低的总生物膜生物量(p<0.05)和较高的死细胞百分比(分别为 44%、52%、52%、79%、42%、43%、62%、65%),高于 GC 和 GC-E(分别为 5%和 1%)。结论是,在实验性复合材料中添加 1.5% NF_TiO 可提高 FS 和 FM,而添加 NbO 颗粒(0.5%、1%、1.5%和 2%)、NF_TiO(1%、1.5%和 2%)和 NbO + NF_TiO 的组合(2%)表现出显著的抗菌效果。