新型氟掺杂纳米氧化锆复合树脂填料的制备及其抗菌性能评价  

Study on synthesis and antibacterial effects on a novel fluoride-doped nano-zirconia composite resin filler

作　　者：郑俪媛 钱超[1] 宁聪琴[2] 孙健[1] Zheng Liyuan;Qian Chao;Ning Congqin;Sun Jian(Department of prosthodontics,Shanghai Ninth People’s Hospital,Shanghai Jiao Tong University School of medicine,College of Stomatology,National Clinical Research Center of Oral Diseases,Shanghai Key Laboratory of Stomatology,Shanghai 200011;Shanghai Institute of Ceramics,Chinese Academy of Sciences,State Key Laboratory of High Performance Ceramics and Super fine Microstructure,Shanghai 200050)

机构地区：[1]上海交通大学医学院附属第九人民医院口腔修复科,上海交通大学口腔医学院,国家口腔医学中心,国家口腔疾病临床医学研究中心,上海市口腔医学重点实验室,上海200011 [2]中国科学院上海硅酸盐研究所,高性能陶瓷和超微结构国家重点实验室,上海200050

出　　处：《口腔材料器械杂志》2021年第4期218-224,共7页Chinese Journal of Dental Materials and Devices

基　　金：高性能陶瓷和超微结构国家重点实验室开放课题基金资助(编号:SKL201909SIC);中华口腔医学会青年科研基金树脂材料研究项目(编号:CSA-R2018-09)。

摘　　要：目的制备一种新型氟掺杂纳米氧化锆复合树脂填料,评价其对口腔变形链球菌的抗菌性能。方法采用化学沉淀和高温煅烧的方法制备得到含氟量为10 mol%和20 mol%的氟掺杂纳米氧化锆粉体(F-ZrO_(2)),并以不含氟纳米氧化锆粉体作为对照组,通过X射线衍射仪(XRD)和扫描电镜(SEM)对以上3组材料的晶相结构及表面形貌进行表征。通过琼脂扩散实验、最小抑菌/杀菌浓度测试和菌落计数实验对其抗菌性能进行定性定量研究。结果不同氟掺杂量的纳米氧化锆粉体表面形貌基本不变,均为球状纳米粉体,粒径分布在15 nm~70 nm之间。氟的掺杂使四方相氧化锆峰值被抑制,单斜相氧化锆峰值逐渐变强。在琼脂扩散实验中,10%F-ZrO_(2)和20%F-ZrO_(2)样品片周围均出现明显抑菌环,测量抑菌环平均直径分别为13.46 mm和16.24 mm。菌落计数结果显示:20%F-ZrO_(2)组、10%F-ZrO_(2)组和0%F-ZrO_(2)组的抑菌率依次为96.79%、82.99%和76.91%,各组间差异具有统计学意义(P<0.05)。结论该氟掺杂纳米氧化锆粉体具备优异的抗菌性能,可作为一种新型复合树脂填料以减少继发龋发生的可能性。Objective The study aimed to synthesize a novel fluoride-doped nano-zirconia composite resin filler by a chemical method and evaluate its antibacterial property against oral Streptococcus mutans(S.mutans).Methods Two groups of fluoride-doped nano-zirconia powders(F-ZrO_(2))with a fluoride content of 10 mol%and 20 mol%were synthesized by chemical precipitation and high-temperature calcination.The fluoride-free nano-zirconia powder was prepared in the same way as a control group here.The crystal phases and the surface morphologies of the above three groups of powders were characterized by scanning electron microscope(SEM)and X-ray diffractometer.Agar-diffusion test,the minimum inhibitory/bactericidal concentration test(MIC/MBC)and colony forming units counting(CFUs)were performed to evaluate the antibacterial property qualitatively and quantitatively.Results The surface morphologies of nano-zirconia powders with different fluoride doping amounts were basically the same,and they were all spherical nanoparticles with sizes ranging from 15 nm to 70 nm.With the increase of fluoride doping,the peaks of tetragonal phase(t phase)zirconia were suppressed gradually and the peak value of monoclinic phase(m phase)zirconia became stronger.In the agar diffusion test,significant bacteriostatic rings were found around 10%F-ZrO_(2) and 20%F-ZrO_(2) samples,with average diameters of 13.46 mm and 16.24 mm respectively.By Counting and calculating the antibacterial rate,the antibacterial effect could be known as:20%F-ZrO_(2)>10%F-ZrO_(2)>0%F-ZrO_(2),with the antibacterial rate of 96.79%,82.99%and 76.91%,respectively.There were statistical differences among groups(P<0.05).Conclusion Fluoride-doped nano-zirconia powder was synthesized successfully,which possessed an excellent antibacterial property and could be used as a new type of composite resin filler to reduce the possibility of secondary caries.

关 键 词：氟化物 纳米氧化锆 复合树脂 填料 抗菌性 

分 类 号：R783.1[医药卫生—口腔医学]