磷酸酸蚀和不同磷酸酯单体预处理牙釉质表面的微观形态学观察和粗糙度评价

›› 2020, Vol. 40 ›› Issue (10): 878-882.

磷酸酸蚀和不同磷酸酯单体预处理牙釉质表面的微观形态学观察和粗糙度评价

韩菲¹,谢海峰¹,陈晨²,石炜³,杨家雪²,景双林³

1. 南京医科大学
2. 南京医科大学附属口腔医院
3. 江苏省口腔医院

收稿日期:2020-04-30 修回日期:2020-06-11 出版日期:2020-10-28 发布日期:2020-10-28
通讯作者: 谢海峰 E-mail:xhf-1980@126.com
基金资助:
国家自然科学基金;江苏省自然科学基金;2019年江苏省青蓝工程优秀青年骨干教师，江苏高校优势学科建设工程资助项目

Micromorphological observation and surface roughness evaluation of enamel surface pretreated by phosphoric acid etching and phosphoric acid ester monomers conditioning

Received:2020-04-30 Revised:2020-06-11 Online:2020-10-28 Published:2020-10-28
Supported by:
National Natural Science Foundation of China;Natural Science Foundation of Jiangsu Province of China;the Qing Lan Project and the Priority Academic Program Development of Jiangsu Higher Education Institutions

摘要/Abstract

摘要： ［摘要］目的探讨磷酸酸蚀不同时间和不同磷酸酯单体预处理对牙釉质表面粗糙度和微观形态的影响。方法切割一定规格的牙釉质试件并以钨钢车针抛光。分别使用35%磷酸酸蚀3、15、30、60 s，含有磷酸酯单体GPDM （glycerol phosphate dimethacrylate）的两步自酸蚀粘结剂Optibond Versa （OV）中的预处理剂和含有磷酸酯单体10-MDP （10-Methacryloyloxydecyl dihydrogen phosphate）的Tetric N Bond Universal（TNBU）进行表面预处理20 s，采用表面轮廓仪测量牙釉质表面粗糙度（Ra），与未处理组（Ctr）做对比，并通过扫描电镜（SEM）观察表面微观形态。结果 35%磷酸酸蚀获得的表面粗糙度最高，其余依次是OV，TNBU和Ctr（P＜0.05）。SEM观察显示，磷酸酸蚀3 s即可见釉柱轻度溶解，酸蚀15 s形成典型的鱼鳞状排列的蜂窝结构，随着酸蚀时间的延长，釉柱间隙愈发明显，釉柱结构出现塌陷。OV预处理剂处理过的牙釉质表面可观察到明显的釉柱边界。TNBU未见明显的釉柱蚀刻表现，划痕仍明显。结论磷酸酸蚀牙釉质时间以15 s为宜，经过磷酸酸蚀和OV预处理剂可以增加牙釉质表面粗糙度。OV预处理剂中的GPDM单体也可使牙釉质表面脱矿且脱矿深度大于TNBU中10-MDP。

关键词: 牙釉质, 磷酸酸蚀时间, 磷酸酯单体, 表面微观形态, 表面粗糙度

Abstract: Objective　 To investigate the effects of different phosphoric acid etching time and conditioning with different phosphoric acid ester monomers on the surface roughness and micromorphology of enamel. Methods　 Enamel samples were prepared with 35% phosphoric acid etching for 3, 15, 30 and 60 seconds, respectively. A two-step self-etch adhesive Optibond Versa (OV) primer containing phosphoric acid ester monomer GPDM (glycerol phosphate dimethacrylate) and Tetric N Bond Universal (TNBU) containing phosphoric acid ester monomer 10-MDP (10-Methacryloyloxydecyl dihydrogen phosphate) were used to pretreat enamel surface for 20 seconds. The enamel surface roughness (Ra), were tested by a profilometer and compared with the untreated group (Ctr) and the surface morphology were observed by scanning electron microscope (SEM). Results　The surface roughness obtained by 35% phosphoric acid etching was the highest, followed by OV, TNBU and Ctr (P＜0.05). SEM showed that the enamel-prism dissolved slightly after phosphoric acid etching for 3 seconds, and the typical fish scale-like honeycomb structure was formed after phosphoric acid etching for 15 seconds. With the extension of phosphoric acid etching time, the gaps between the enamel-prisms became more obvious and the enamel-prism structure collapsed. The obvious enamel-prism contours can be observed on the enamel surface treated with OV primer. There was no obvious enamel-prism etching in TNBU, and the scratches were still clear. Conclusions　15 seconds phosphoric acid etching of enamel is recommended. Enamel surface roughness can be increased by phosphoric acid etching and GPDM-containing primer conditioning. GPDM-containing primer achieved higher demineralization depth than that of 10-MDP containing adhesive.

Key words: enamel, phosphoric acid etching time, phosphoric acid ester monomers, micromorphology, surface roughness

中图分类号:

R783.1

韩菲谢海峰陈晨石炜杨家雪景双林. 磷酸酸蚀和不同磷酸酯单体预处理牙釉质表面的微观形态学观察和粗糙度评价[J]. 口腔医学, 2020, 40(10): 878-882.

参考文献 20

[1]	Wong J, Tsujimoto A, Fischer NG, et al. Enamel Etching for Universal Adhesives: Examination of Enamel Etching Protocols for Optimization of Bonding Effectiveness [J]. Oper Dent, 2020, 45(1)：80–91.
[2]	Takeda M, Takamizawa T, Imai A, et al. Immediate enamel bond strength of universal adhesives to unground and ground surfaces in different etching modes [J]. Eur J Oral Sci, 2019, 127(4)：351–360.
[3]	Barkmeier WW, Erickson RL, Kimmes NS, et al. Effect of enamel etching time on roughness and bond strength [J]. Oper Dent, 2009, 34(2)：217–222.
[4]	Suzuki S, Takamizawa T, Imai A, et al. Bond durability of universal adhesive to bovine enamel using self-etch mode [J]. Clin Oral Investig, 2018, 22(3)：1113–1122.
[5]	Yao C, Ahmed MH, Yoshihara K, et al. Bonding to enamel using alternative Enamel Conditioner/etchants [J]. Dent Mater, 2019, 35(10)：1415–1429.
[6]	Shimatani Y, Tsujimoto A, Nojiri K, et al. Reconsideration of Enamel Etching Protocols for Universal Adhesives: Effect of Etching Method and Etching Time [J]. J Adhes Dent, 2019, 21(4)：345–354.
[7]	Giannini M, Makishi P, Ayres AP, et al. Self-etch adhesive systems: a literature review [J]. Braz Dent J, 2015, 26(1)：3–10.
[8]	Makishi P, André CB, Ayres A, et al. Effect of Storage Time on Bond Strength and Nanoleakage Expression of Universal Adhesives Bonded to Dentin and Etched Enamel [J]. Oper Dent, 2016, 41(3)：305–317.
[9]	Yoshihara K, Nagaoka N, Hayakawa S, et al. Chemical interaction of glycero-phosphate dimethacrylate (GPDM) with hydroxyapatite and dentin [J]. Dent Mater, 2018, 34(7)：1072–1081.
[10]	De Menezes Oliveira MA, Torres CP, Gomes-Silva JM, et al. Microstructure and mineral composition of dental enamel of permanent and deciduous teeth [J]. Microsc Res Tech, 2010, 73(5)：572–577.
[11]	Tsujimoto A, Fischer N, Barkmeier W, et al. Effect of Reduced Phosphoric Acid Pre-etching Times on Enamel Surface Characteristics and Shear Fatigue Strength Using Universal Adhesives [J]. J Adhes Dent, 2017, 19(3)：267–275.
[12]	Tsujimoto A, Barkmeier WW, Erickson RL, et al. Influence of the number of cycles on shear fatigue strength of resin composite bonded to enamel and dentin using dental adhesives in self-etching mode [J]. Dent Mater J, 2018, 37(1)：113–121.
[13]	Barkmeier WW, Shaffer SE, Gwinnett AJ. Effects of 15 vs 60 second enamel acid conditioning on adhesion and morphology [J]. Oper Dent, 1986, 11(3)：111–116.
[14]	Suda S, Tsujimoto A, Barkmeier WW, et al. Comparison of enamel bond fatigue durability between universal adhesives and two-step self-etch adhesives: Effect of phosphoric acid pre-etching [J]. Dent Mater J, 2018, 37(2)：244–255.
[15]	Zafar MS, Ahmed N. The effects of acid etching time on surface mechanical properties of dental hard tissues [J]. Dent Mater J, 2015, 34(3)：315–320.
[16]	Tsuchiya K, Takamizawa T, Barkmeier WW, et al. Effect of a functional monomer (MDP) on the enamel bond durability of single-step self-etch adhesives [J]. Eur J Oral Sci, 2016, 124(1)：96–102.
[17]	Yoshihara K, Hayakawa S, Nagaoka N, et al. Etching Efficacy of Self-Etching Functional Monomers [J]. J Dent Res, 2018, 97(9)：1010–1016.
[18]	Wang C, Zhao Y, Zheng S, et al. Effect of enamel morphology on nanoscale adhesion forces of streptococcal bacteria : An AFM study [J]. Scanning, 2015, 37(5)：313–321.
[19]	Lawson NC, Robles A, Fu CC, et al. Two-year clinical trial of a universal adhesive in total-etch and self-etch mode in non-carious cervical lesions [J]. J Dent, 2015, 43(10)：1229–1234.
[20]	Hoshika S, Kameyama A, Suyama Y, et al. GPDM- and 10-MDP-based Self-etch Adhesives Bonded to Bur-cut and Uncut Enamel - "Immediate" and "Aged" μTBS [J]. J Adhes Dent, 2018, 20(2)：113–120.