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中华口腔医学研究杂志(电子版) ›› 2021, Vol. 15 ›› Issue (05) : 284 -291. doi: 10.3877/cma.j.issn.1674-1366.2021.05.005

基础研究

不同酸蚀模式对新型窝沟封闭剂在牙釉质表面粘接耐久性的影响
王万锋1, 徐正一2, 李家硕1, 曾祥隽1, 龚兆威1, 战德松3, 付佳乐3,†()   
  1. 1. 中国医科大学口腔医学院，沈阳　110002
    2. 四川大学华西口腔医学院修复科，口腔疾病研究国家重点实验室，国家口腔疾病临床医学研究中心，成都　610041
    3. 中国医科大学口腔医学院口腔材料学教研室，中国医科大学附属口腔医院修复二科，沈阳　110002
  • 收稿日期:2021-07-23 出版日期:2021-10-01
  • 通信作者: 付佳乐

Effect of different etching modes on the bonding durability of a new pit and fissure sealant on enamel surface

Wanfeng Wang1, Zhengyi Xu2, Jiashuo Li1, Xiangjun Zeng1, Zhaowei Gong1, Desong Zhan3, Jiale Fu3,†()   

  1. 1. School of Stomatology, China Medical University, Shenyang 110002, China
    2. Department of Prosthetics, West China Hospital of Stomatology, Sichuan University, State Key Laboratory of Oral Diseases, National Clinical Research Center for Oral Diseases, Chengdu 610041, China
    3. Department of Dental Materials, China Medical University School of Stomatology, Department of Prosthodontics, China Medical University Hospital of Stomatology, Shenyang 110002, China
  • Received:2021-07-23 Published:2021-10-01
  • Corresponding author: Jiale Fu
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引用本文：

王万锋, 徐正一, 李家硕, 曾祥隽, 龚兆威, 战德松, 付佳乐. 不同酸蚀模式对新型窝沟封闭剂在牙釉质表面粘接耐久性的影响[J]. 中华口腔医学研究杂志(电子版), 2021, 15(05): 284-291.

Wanfeng Wang, Zhengyi Xu, Jiashuo Li, Xiangjun Zeng, Zhaowei Gong, Desong Zhan, Jiale Fu. Effect of different etching modes on the bonding durability of a new pit and fissure sealant on enamel surface[J]. Chinese Journal of Stomatological Research(Electronic Edition), 2021, 15(05): 284-291.

目的

研究37 ℃水浴24 h及冷热循环5000次条件下，人离体牙釉质表面不同酸蚀模式对一种新型窝沟封闭剂粘接强度及耐久性的影响。

方法

选择健康无龋的人离体第三磨牙30颗，暴露牙釉质平面，最终得到24个离体牙试件。将试件按随机数字表法分为2组（n = 12），再根据不同的酸蚀模式分为磷酸组（A组）、通用型粘接剂组（B组）和磷酸+通用型粘接剂组（C组）3个亚组（n = 4）。按照不同酸蚀模式进行操作后，试件分别在37 ℃恒温水浴24 h与冷热循环5000次后进行剪切强度测试。实验数据采用SPSS 22.0进行三因素分析（存储条件、酸蚀模式与窝沟封闭剂颜色）并用单因素分析Turkey或Games-Howell对结果进行统计学处理。利用显微镜进行牙釉质端的断裂模式分析并进行扫描电镜观察与能谱分析。

结果

37 ℃水浴24 h后，C组封闭剂的剪切结合强度（SBS）为（22.18 ± 4.55）MPa，显著高于A组[（16.07 ± 4.17）MPa]和B组[（16.40 ± 3.01）MPa]，差异均有统计学意义（FA组 = 11.779，PA组 = 0.002；FB组 = 13.436，PB组 = 0.001），A组与B组间SBS差异无统计学意义（F = 0.068，P = 0.797）；在冷热循环5000次后，A组的SBS为（12.69 ± 3.00）MPa，B组为（0.00 ± 0.00）MPa，C组为（12.17 ± 2.85）MPa，各组SBS均出现下降，其中A组的下降差异无统计学意义（F = 1.504，P = 0.225），而B组和C组的下降差异有统计学意义（FB组 = 165.896，PB组<0.001；FC组 = 51.665，PC组<0.001），A组与C组间SBS差异无统计学意义（F = 0.182，P = 0.674），但均显著高于B组（FA组 = 213.353，PA组<0.001；FC组 = 219.470，PC组<0.001）。三因素方差分析结果显示，三者交互作用差异无统计学意义（F = 1.376，P = 0.254）。断裂模式分析显示，冷热循环5000次后Ⅱ类断裂模式显著增加，B组未出现釉柱断裂，C组釉柱断裂的减少程度大于A组。

结论

磷酸+通用型粘接剂能显著提高窝沟封闭剂在牙釉质表面37 ℃水浴24 h的粘接强度；而磷酸酸蚀处理牙釉质后使用窝沟封闭剂的耐久性更优。

关键词: 窝沟封闭, 牙科酸蚀, 表面处理, 剪切强度, 耐久性
Objective

To compare the effect of different etching modes on the bond strength and durability of a new type of pit and fissure sealant on the surface of human enamel in vitro after storage in water (37 ℃) for 24 h and thermocycling for 5000 times.

Methods

In the present study, a total of 30 caries-free human third molars were selected and the enamel plane was exposed, of which 24 specimens were used for this experiment. The specimens were divided into two groups according to random number table method (n = 12) , and further divided into 3 subgroups (n = 4) according to different etching modes: phosphoric acid group (group A) , universal adhesive group (group B) and phosphoric acid + universal adhesive group (group C) . After specimen preparation, the shear bond strength (SBS) test was carried out after 37 ℃ water storage for 24 h and after thermocycling for 5000 times, respectively. The data from SBS were analyzed by using Three-Way ANOVA (storage condition, etching mode and color of pit and fissure sealant) , and Turkey/Games-Howell (α = 0.05) . The fracture mode was analyzed by light microscope and fracture surface on enamel was observed by scanning electron microscope (SEM) with the application of energy spectroscopy.

Results

After storage in 37 ℃ water for 24 h, the SBS of group C was (22.18 ± 4.55) MPa, which was significantly higher than that of group A (16.07 ± 4.17) MPa (F = 11.779, P = 0.002) and group B (16.40 ± 3.01) MPa (F = 13.436, P = 0.001) . No significant difference was detected between group A and group B (F = 0.068, P = 0.797) . After thermocycling for 5000 times, the SBS of group A was (12.69 ± 3.00) MPa, that of group B was (0.00 ± 0.00) MPa, and group C was (12.17 ± 2.85) MPa, all of which decreased. There was no statistical difference in the change of SBS in group A (F = 1.504, P = 0.225) , whereas significant decrease was found in group B and C (FB group = 165.896, PB group<0.001; FC group = 51.665, PC group<0.001) . No statistical difference was found between group A and group C (F = 0.182, P = 0.674) , both of which were significantly higher than that of group B (FA group = 213.353, PA group<0.001; FC group = 219.470, PC group<0.001) . Three-Way ANOVA analysis of variance revealed that the interaction within these three factors was not statistically significant (F = 1.376, P = 0.254) . After thermocycling for 5000 times, the type Ⅱ fracture mode was significantly increased, but no enamel prisms fracture was detected in group B. The downtrend of enamel prisms fracture in group C was greater than that in group A.

Conclusions

The bond strength of pit and fissure sealant on enamel could be significantly enhanced by the combination of phosphoric acid etching and universal adhesive after storage in 37 ℃ water for 24 h. The durability of pit and fissure sealant after acid etching of dental enamel was improved.

Key words: Pit and fissure sealant, Dental etching, Surface treatment, Shear strength, Durability
表1 本研究使用窝沟封闭剂的结构组成
类别 结构组成
1.甲基丙烯酸酯类单体 二-2-甲基丙烯酸酰氧乙基-2，2，4-三甲基己烷二氨基甲酸酯；1，6-己二醇二甲基丙烯酸酯；双酚A二缩水甘油二甲基丙烯酸酯
2.无机填料 锶玻璃粉、钡玻璃粉、硅粉
3.光引发剂 樟脑醌
4.稳定剂 对羟基苯甲醚
5.颜料 氧化铁；某蓝色无机颜料
图1 实验分组流程图　SBS为剪切结合强度
表2 酸蚀模式、颜色和储存条件3个变量的三因素方差分析结果
方差来源 平方和 自由度 均方 F值 P值
酸蚀模式 761.161 2 380.581 41.761 0.000
颜色 41.457 2 20.729 2.275 0.113
储存条件 1270.712 1 1270.712 139.433 0.000
酸蚀模式*颜色 139.486 4 34.871 3.826 0.008
酸蚀模式*储存条件 525.127 2 262.564 28.811 0.000
颜色*储存条件 9.904 2 4.952 0.543 0.584
酸蚀模式*颜色*储存条件 50.159 4 12.540 1.376 0.254
表3 3组试件剪切结合强度（SBS）试验的统计学分析结果（MPa，±s）
组别 试件数 24 h 5000次
A组 4 16.07 ± 4.17Aa 12.69 ± 3.00Aa
B组 4 16.40 ± 3.01Aa 0.00 ± 0.00Bb
C组 4 22.18 ± 4.55Ab 12.17 ± 2.85Ba
图2 3组试件剪切结合强度（SBS）测试后各组断裂模式统计图
图3 5000次冷热循环后各组试件的粘接界面扫描电镜观察　A：A组；B：B组；C：C组；D：A图方框放大图；E：B图方框放大图；F：C图方框放大图；白色箭头：残留的粘接剂；黑色箭头：砂纸打磨后的釉质表面；红色箭头：釉质断裂处
图4 5000次冷热循环后各组试件的粘接界面扫描电镜（SEM）能谱分析图　A：A组SEM观察；B~D：分别为A组能谱分析硅元素（Si）、磷元素（P）、钙元素（Ca）的分布情况；E：B组SEM观察；F：NA表示B组试件未检测出Si；G~H：分别为B组能谱分析P、Ca的分布情况；J：C组SEM观察；K~I：分别为C组能谱分析Si、P、Ca的分布情况
图5 实验所用窝沟封闭剂光固化后的向光性聚合收缩现象　A：光照前；B：光照中；C：光照后；图中所用离体牙试件的牙本质已暴露，为废弃试件
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