Department of Prosthodontics, College of Dentistry, Yonsei University, 50-1 Yonsei-ro, Seodaemun-gu, Seoul 03722, Republic of Korea.
Division of Bioengineering, Incheon National University, Incheon 22012, Republic of Korea.
J Dent. 2024 Nov;150:105363. doi: 10.1016/j.jdent.2024.105363. Epub 2024 Sep 28.
To synthesize a 3D printing resin with antibacterial and long-term fluoride-releasing properties.
(4,4-Bis-4-[2‑hydroxy-3-(2-methacryloyloxy)propoxy]-phenyl-pentanol-amine)-N,N-diacetic acid zirconium (IV) fluoride complex was synthesized from 4,4-bis-(4-hydroxyphenyl)-pentanoic acid and monitored using proton nuclear magnetic resonance spectroscopy. The synthesized complex was incorporated into a urethane-acrylate-based (UA) resin at 5 wt% and 10 wt% (5F-UA and 10F-UA groups, respectively). The UA resin without the synthesized complex was considered as the control group. All groups were 3D printed using a DLP printer, followed by 10 min of washing and 20 min of curing. Surface characteristics were observed using scanning electron microscopy. The mechanical properties were assessed by measuring its flexural strength and Vickers hardness. The antibacterial property was investigated with direct and indirect contact tests and a WST-8 metabolic activity assay. The suspension was fully mixed and diluted for counting the number of colony-forming units. The cell viability test was performed using a cell proliferation assay. The amount of fluoride released was measured daily for 28 days using ion chromatography. One-way analysis of variance was performed for statistical analyses using SPSS software.
The amount of fluoride released increased with the concentration of fluoride complex in the resin. The fluoride ions were constantly released at a low concentration from the 3D printed specimens (5F-UA: around 0.13 ppm daily; 10F-UA: around 0.22 ppm daily). The antibacterial efficacy was acceptable in both the 5F-UA and 10F-UA groups, and higher in the latter. No cytotoxicity of the resin was detected. The mechanical properties were significantly influenced by the addition of the fluoride-releasing complex.
The present 3D printing UA resin incorporating a fluoride complex effectively inhibited the growth of S. mutans and demonstrated the ability to slowly release fluoride over an extended period of time.
This study provided informative composition of a fluoride-releasing UA-based 3D printing resin, ideal for dental applications such as crowns, bridges, removable partial dentures, and orthodontic appliances, which can benefit from sustained fluoride release and antimicrobial properties. Further modifications to the resin composition can be easily achieved to enhance the resin qualities.
合成一种具有抗菌和长期氟释放性能的 3D 打印树脂。
(4,4-双-(4-[2-羟基-3-(2-甲丙烯酰氧基)丙氧基]苯基)戊基-胺)-N,N-二乙酸锆(IV)氟络合物由 4,4-双-(4-羟苯基)戊酸合成,并通过质子核磁共振光谱进行监测。将合成的络合物以 5wt%和 10wt%(5F-UA 和 10F-UA 组)的比例掺入到基于氨酯丙烯酸酯(UA)的树脂中。不含合成络合物的 UA 树脂被认为是对照组。所有组均使用 DLP 打印机进行 3D 打印,然后进行 10 分钟的清洗和 20 分钟的固化。使用扫描电子显微镜观察表面特性。通过测量其弯曲强度和维氏硬度来评估机械性能。通过直接和间接接触试验以及 WST-8 代谢活性测定法研究抗菌性能。将悬浮液充分混合并稀释,以计数菌落形成单位的数量。使用细胞增殖测定法进行细胞活力测试。使用离子色谱法每天测量 28 天内释放的氟化物量。使用 SPSS 软件进行单向方差分析进行统计分析。
释放的氟化物量随树脂中氟络合物浓度的增加而增加。氟离子从 3D 打印标本中以低浓度持续释放(5F-UA:每天约 0.13ppm;10F-UA:每天约 0.22ppm)。5F-UA 和 10F-UA 组的抗菌效果均可以接受,后者更高。未检测到树脂的细胞毒性。机械性能受添加释放氟化物的复合物的影响显著。
本研究中,掺入氟释放复合物的 3D 打印 UA 树脂有效抑制了变形链球菌的生长,并表现出在较长时间内缓慢释放氟化物的能力。
本研究提供了一种基于 UA 的含氟释放 3D 打印树脂的组成信息,非常适合于牙冠、牙桥、可摘局部义齿和正畸矫治器等牙科应用,可受益于持续释放氟化物和抗菌性能。可以通过对树脂成分进行简单的修改来增强树脂的性能。