Han Fei, Dai Shiqi, Yang Jiaxue, Shen Jiadi, Liao Mengyuan, Xie Haifeng, Chen Chen
Jiangsu Key Laboratory of Oral Diseases; Department of Prosthodontics, Affiliated Hospital of Stomatology, Nanjing Medical University, Nanjing 210029, China.
Jiangsu Key Laboratory of Oral Diseases; Department of Endodontics, Affiliated Hospital of Stomatology, Nanjing Medical University, Nanjing 210029, China.
ACS Omega. 2020 Sep 17;5(38):24826-24837. doi: 10.1021/acsomega.0c03523. eCollection 2020 Sep 29.
The bonding performance of a glycerol phosphate dimethacrylate (GPDM)-based, two-step, self-etch (SE) adhesive was experimentally compared to that of 10-methacryloyloxydecyl dihydrogen phosphate (MDP)-based universal adhesives in different application modes for enamel bonding. Microtensile bond strength (μTBS) for adhesives bonded to enamel was measured initially (24 h water storage) and after 10 000 thermocycles plus water storage for 30 days. A GPDM-based, two-bottle, two-step, self-etch adhesive (Optibond Versa, OV) and three one-bottle MDP-based universal adhesives, one self-etching (Tetric N Bond Universal, TNBU) and two with etch-and-rinse (E&R) processing (Single Bond Universal (SBU); Clearfil Universal Bond Quick (CUBQ)), were tested. Scanning electron microscopy (SEM) evaluated nanoleakage at the bonding interfaces. A profilometer determined roughnesses of enamel surfaces after phosphoric acid etching, OV priming, or TNBU conditioning. SEM observed the corresponding surface morphology. NMR and X-ray photoelectron spectroscopy (XPS) characterized chemical bonding in hydroxyapatites (HAps) conditioned with the adhesives. Etch-and-rinse samples had significantly stronger bonding than self-etch samples ( < 0.05) irrespective of aging. The μTBS values for initial and aged OV were significantly higher than those of TNBU ( < 0.05). Aging did not significantly decrease μTBS for any sample except TNBU ( < 0.05), but it significantly aggravated nanoleakage. Etch-and-rinse processing resulted in less nanoleakage than self-etching; the OV samples leaked less than TNBU, both before and after aging. Phosphoric acid etching achieved the highest enamel surface roughness, followed by OV primer. Ca-O-P bonds in hydroxyapatite conditioned with TNBU, SBU, and CUBQ were confirmed by NMR, which showed similar results to XPS observations of conditioned hydroxyapatite powders except OV primer. The GPDM-based, two-step, self-etch adhesive can provide higher micromechanical retention potential, bond strength, and durability than the MDP-based universal adhesive in self-etch mode but lower performance than the MDP-based universal adhesive in etch-and-rinse mode. None of the tested adhesives could avoid nanoleakage after aging.
实验比较了基于磷酸甘油二甲基丙烯酸酯（GPDM）的两步自酸蚀（SE）粘合剂与基于10-甲基丙烯酰氧基癸基磷酸二氢酯（MDP）的通用粘合剂在不同牙釉质粘结应用模式下的粘结性能。最初（储存24小时水后）以及经过10000次热循环加30天储水后，测量粘合剂与牙釉质粘结的微拉伸粘结强度（μTBS）。测试了一种基于GPDM的双瓶装两步自酸蚀粘合剂（Optibond Versa，OV）和三种基于MDP的单瓶装通用粘合剂，一种自酸蚀型（Tetric N Bond Universal，TNBU）以及两种酸蚀冲洗（E&R）型（Single Bond Universal（SBU）；Clearfil Universal Bond Quick（CUBQ））。扫描电子显微镜（SEM）评估粘结界面处的纳米渗漏情况。轮廓仪测定磷酸酸蚀、OV涂底或TNBU预处理后牙釉质表面的粗糙度。SEM观察相应的表面形态。核磁共振（NMR）和X射线光电子能谱（XPS）表征用粘合剂处理过的羟基磷灰石（Haps）中的化学键合情况。无论老化与否，酸蚀冲洗型样品的粘结力均显著强于自酸蚀型样品（<0.05）。初始和老化后的OV的μTBS值显著高于TNBU（<0.05）。除TNBU外（<0.05），老化对任何样品的μTBS均无显著降低作用，但显著加剧了纳米渗漏。酸蚀冲洗处理导致的纳米渗漏少于自酸蚀处理；老化前后，OV样品的渗漏均少于TNBU。磷酸酸蚀使牙釉质表面粗糙度最高，其次是OV涂底剂。通过NMR证实了用TNBU、SBU和CUBQ处理过的羟基磷灰石中的Ca-O-P键，其结果与除OV涂底剂外的处理过的羟基磷灰石粉末的XPS观察结果相似。基于GPDM的两步自酸蚀粘合剂在自酸蚀模式下比基于MDP的通用粘合剂能提供更高的微机械固位潜力、粘结强度和耐久性，但在酸蚀冲洗模式下性能低于基于MDP的通用粘合剂。老化后，所测试的粘合剂均无法避免纳米渗漏。
