Biomaterial and Biomedical Sciences Division, School of Dentistry, Oregon Health & Science University, 2730 S Moody Ave, Portland, Oregon 97201, United States.
Dental Materials, Piracicaba School of Dentistry, University of Campinas, Av. Limeira, 901, Piracicaba, SP 13414-903, Brazil.
ACS Appl Mater Interfaces. 2024 Sep 4;16(35):46005-46015. doi: 10.1021/acsami.4c07960. Epub 2024 Aug 23.
Acrylamides are hydrolytically stable at pH lower than 2, and were shown to preserve bonded interface integrity with two-step, total etch adhesives. The objective of this study was to leverage those two characteristics in self-etching primers containing the acidic monomer 10-MDP and test the microtensile bond strength before and after incubation with incubation. Acidic primers (10 wt % 10-methacryloyloxydecyl dihydrogen phosphate─10-MDP; 45 wt % ,-diethyl-1,3-bis(acrylamido)propane─DEBAAP, or 2-hydroxyethyl methacrylate─HEMA; 45 wt %, glycerol-dimethacrylate─GDMA) and adhesives (DEBAAP or HEMA/10-MDP/UDMA 45/10/45 wt %) were made polymerizable by the addition of 0.2 wt % camphorquinone, 0.8 wt % ethyl-4-dimethylaminobenzoate, 0.4 wt % diphenyliodonium hexafluorophosphate, and 0.1 wt % butylhydroxytoluene. Nonsolvated materials were characterized for flexural strength (FS), modulus (E), toughness, water sorption/solubility (WS/SL), contact angle, and vinyl conversion (DC). Viscosity was evaluated after adding 20 and 40 vol % ethanol to the primer and adhesive, respectively. The experimental materials or Clearfil SE Bond (CC─commercial control) were used to bond a commercial composite (Filtek Supreme) to the flat surface of human dentin. Microtensile bond strength (MTBS) was tested in 1 mm sticks for the 5 primer/bond combinations: CC (Clearfil Bond Primer and Bond), HH (HEMA/HEMA), DD (DEBAAP/DEBAAP), HD (HEMA/DEBAAP), and DH (DEBAAP/HEMA). Prior to testing, sticks were stored in water or biofilm-inducing culture medium with for 1 week. Confocal images and FTIR-ATR evaluation evaluated the hybrid layer of the adhesives. Results were analyzed using Student's -test (WS, SL, DC, contact angle, FS, E, toughness), one-way ANOVA/Tukey's test for viscosity, and two-way ANOVA/Tukey's test for MTBS (95%). HEMA-based materials had lower contact angle ( = 0.004), higher WS ( < 0.001), and similar SL values compared to DEBAAP ( = 0.126). FS ( = 0.171) and E ( = 0.065) dry values were similar, but after one week of water storage, FS/E dropped more significantly for HEMA materials. Dry and wet toughness was greater for DEBAAP ( < 0.001), but it also had the greatest drop (46%). Clearfil bonds had the highest viscosity, followed by DEBAAP and HEMA, respectively ( = 0.002). For the primers, HEMA had the lowest viscosity ( = 0.003). As far as MTBS, all groups tested in water were statistically different when compared with HH ( < 0.001). After storage in biofilm, DH had the highest MTBS value, being statistically different from HH ( = 0.002), CC ( = 0.015), and DD ( = 0.027). The addition of a diacrylamide and its association with HEMA in self-etching adhesive systems provided greater bonding stability after bacterial challenge.
丙烯酰胺在 pH 值低于 2 时水解稳定,并被证明可以保持两步全蚀刻黏合剂的键合界面完整性。本研究的目的是利用这两个特性,在含有酸性单体 10-MDP 的自酸蚀底漆中进行测试,并在孵育后测试微拉伸黏结强度。酸性底漆(10 wt % 10-丙烯酰氧基癸基二氢磷酸酯-10-MDP;45 wt % ,-二乙基-1,3-双(丙烯酰胺基)丙烷-DEBAAP 或 2-羟乙基甲基丙烯酸酯-HEMA;45 wt %,甘油二甲基丙烯酸酯-GDMA)和黏合剂(DEBAAP 或 HEMA/10-MDP/UDMA 45/10/45 wt %)通过添加 0.2 wt %樟脑醌、0.8 wt %乙基-4-二甲氨基苯甲酸酯、0.4 wt %二苯基碘𬭩六氟磷酸盐和 0.1 wt %丁基羟基甲苯而具有聚合性。未溶剂化材料的弯曲强度(FS)、模量(E)、韧性、吸水率/溶解度(WS/SL)、接触角和乙烯基转化率(DC)进行了表征。在分别向底漆和黏合剂中添加 20 和 40 体积 %乙醇后,评估了其黏度。实验材料或 Clearfil SE Bond(CC─商业对照)被用于将商业复合材料(Filtek Supreme)黏合到人的牙本质的平面上。使用 5 种底漆/黏合剂组合(CC、HH、DD、HD、DH)在 1mm 棒上进行微拉伸黏结强度(MTBS)测试:CC(Clearfil Bond Primer 和 Bond)、HH(HEMA/HEMA)、DD(DEBAAP/DEBAAP)、HD(HEMA/DEBAAP)和 DH(DEBAAP/HEMA)。在测试之前,将棒储存在水中或含有生物膜诱导培养基中 1 周。使用共聚焦显微镜图像和 FTIR-ATR 评估评估黏合剂的混合层。使用学生 t 检验(WS、SL、DC、接触角、FS、E、韧性)、单因素方差分析/Tukey 检验(黏度)和双因素方差分析/Tukey 检验(MTBS(95%))分析结果。与 DEBAAP 相比,基于 HEMA 的材料具有更低的接触角( = 0.004)、更高的 WS( < 0.001)和相似的 SL 值( = 0.126)。干燥状态下的 FS( = 0.171)和 E( = 0.065)值相似,但在一周的水储存后,HEMA 材料的 FS/E 下降更为显著。干燥和湿态韧性对 DEBAAP 更高( < 0.001),但它的降幅也最大(46%)。Clearfil 黏合剂的黏度最高,其次是 DEBAAP 和 HEMA( = 0.002)。对于底漆,HEMA 的黏度最低( = 0.003)。就 MTBS 而言,与 HH 相比,所有在水中测试的组都具有统计学差异( < 0.001)。在生物膜储存后,DH 的 MTBS 值最高,与 HH ( = 0.002)、CC ( = 0.015)和 DD ( = 0.027)相比具有统计学差异。在自酸蚀黏合剂系统中添加二丙烯酰胺及其与 HEMA 的结合为细菌挑战后的黏合稳定性提供了更大的保障。