水中浸泡对自修复抗菌复合树脂性能影响的实验研究

doi:10.7518/hxkq.2018.05.011

华西口腔医学杂志 ›› 2018, Vol. 36 ›› Issue (5): 521-527.doi: 10.7518/hxkq.2018.05.011

水中浸泡对自修复抗菌复合树脂性能影响的实验研究

吴峻岭¹(),李彤²,高旭¹,张强³(),刘迪¹,葛建华⁴,周传健⁴

^1. 山东大学口腔医学院口腔修复学教研所,山东省口腔组织再生重点实验室,济南 250012
^2. 济南市口腔医院牙体牙髓科
^3. 济南市口腔医院口腔种植诊疗中心,济南 250001
^4. 山东大学材料科学与工程学院高分子材料研究所,济南 250061

收稿日期:2018-03-23 修回日期:2018-06-10 出版日期:2018-10-01 发布日期:2018-10-18
作者简介:吴峻岭,副主任医师,博士,E-mail： doctorwujunling@163.com
基金资助:
国家自然科学基金面上项目(81671032);山东省自然科学基金面上项目(ZR2014HM047)

Effect of water immersion on a dental self-healing and antibacterial resin composite

Junling Wu¹(),Tong Li²,Xu Gao¹,Qiang Zhang³(),Di Liu¹,Jianhua Ge⁴,Chuanjian Zhou⁴

^1. Dept. of Prosthodontics, School of Stomatology, Shandong Uni-versity, Shandong Provincial Key Laboratory of Oral Tissue Regeneration, Jinan 250012, China
^2. Dept. of Conservative Dentistry and Endodontics, Jinan Stomatological Hospital, Jinan 250001, China
^3. Oral Implantology Center, Jinan Sto-matological Hospital, Jinan 250001, China
^4. Research Institute of Polymer Materials, School of Materials Science and Engineering, Shandong University, Jinan 250061, China

Received:2018-03-23 Revised:2018-06-10 Online:2018-10-01 Published:2018-10-18
Supported by:
The National Natural Science Foundation of China(81671032);Shandong Natural Science Foundation Project(ZR2014HM047)

摘要/Abstract

摘要：

目的合成新型牙科自修复抗菌复合树脂,并探讨水中浸泡对其相关性能的影响。方法在前期研究的基础上,制备含牙科自修复单体三乙二醇二甲基丙烯酸酯的微胶囊,以7.5%的质量百分比添加到含长链烷基季铵盐修饰的纳米抗菌二氧化硅填料的复合树脂中,生成自修复抗菌复合树脂,并以商品化的Tetric N-Ceram纳米瓷化复合树脂作为对照。复合树脂试件在37 ℃蒸馏水中浸泡处理不同时间,用三点弯曲试验来检测其力学性能;用单刃V形切口梁法来测试其断裂韧性及自修复效率;建立人牙菌斑生物膜体外模型,通过菌落计数、乳酸代谢分析等手段来评价其抗菌性能。结果浸泡30 d后,对照组和实验组所有复合树脂力学性能及断裂韧性下降明显（P<0.05）,而后随着浸泡时间的延长,下降不明显（P>0.05）;水浸泡处理对自修复效率没有明显影响（P>0.05）,浸泡270 d后仍然可以获得64%的自修复效率;随着浸泡时间的延长,与对照组相比,实验组复合树脂对人牙菌斑生物膜的代谢仍然可以产生明显的抑制作用（P<0.05）,而实验组各时间段之间菌落计数及乳酸产生量则没有明显差异（P>0.05）,显示出良好的抗菌性能。结论水中浸泡可以明显影响自修复抗菌复合树脂的力学性能,而自修复特性及抗菌性能则没有明显的变化。

关键词: 水中浸泡, 微胶囊, 自修复, 抗菌性, 复合树脂

Abstract:

Objective This investigation aimed to develop a novel self-healing and antibacterial dental resin composite. The effects of water immersion on its properties were also evaluated. Methods Microcapsules filled with healing agent of triethylene glycol dimethacrylate were synthesized on the basis of previous studies. Antibacterial resin composite contained nano-antibacterial inorganic fillers that were modified by quaternary ammonium salt with long-chain alkyl. Microcapsules were incorporated into antibacterial resin composite at mass fraction of 7.5%. A commercial resin composite named Tetric N-Ceram was used as control. The resin samples were immersed in 37 °C distilled water for different periods. A flexural test was used to measure the mechanical properties of the novel resin composite. A single-edge V-notched beam method was used to measure fracture toughness and self-healing efficiency. A dental plaque microcosm biofilm model with human saliva as inoculum was formed. Colony-forming units (CFU) and lactic acid production of biofilm on the novel resin composite were calculated to test the antibacterial property. Results Mechanical properties and fracture toughness decreased significantly after the composite was immersed in water for 30 days (P<0.05), and no significant reduction was found from then on (P>0.05). Water immersion did not weaken the self-healing capability of the composite (P>0.05), and self-healing efficiency of 64% could still be obtained even after 270 days. The antibacterial resin composite showed a strong inhibition effect on the biofilm metabolic activity versus water immersion time from 1 day to 270 days. Therefore, the com-posite could still have a promising antibacterial property even after being immersed in water (P<0.05). Conclusion Water immersion could weaken the mechanical properties of the novel self-healing and antibacterial resin composite, but it insig-nificantly affected the self-healing and antibacterial properties of the composite.

Key words: water immersion, microcapsule, self-healing, antibacterial property, resin composite

中图分类号:

R783

吴峻岭,李彤,高旭,张强,刘迪,葛建华,周传健. 水中浸泡对自修复抗菌复合树脂性能影响的实验研究[J]. 华西口腔医学杂志, 2018, 36(5): 521-527.

Junling Wu,Tong Li,Xu Gao,Qiang Zhang,Di Liu,Jianhua Ge,Chuanjian Zhou. Effect of water immersion on a dental self-healing and antibacterial resin composite[J]. West China Journal of Stomatology, 2018, 36(5): 521-527.

图/表 5

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表 1

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图 2

表 3

参考文献 15

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组别	观测时间/d	弯曲强度/MPa	弹性模量/GPa
对照组	1	100±16^a	6.2±0.9^a
	30	69±12^b	4.3±0.7^b
	90	70±11^b	4.3±0.7^b
	180	70±10^b	4.2±0.6^b
	270	69±11^b	4.1±0.7^b
实验组	1	95±13^a	6.1±1.1^a
	30	67±11^b	4.0±0.8^b
	90	69±10^b	4.1±0.7^b
	180	70±8^b	4.3±0.7^b
	270	70±12^b	4.2±0.8^b

组别	观测时	K_IC-virgin/	K_IC-healed/	自修复效
组别	间/d	（MPa·m^1/2）	（MPa·m^1/2）	率η/%
对照组	1	1.2±0.2^a	0	0
	30	0.8±0.2^b	0	0
	90	0.8±0.1^b	0	0
	180	0.7±0.1^b	0	0
	270	0.7±0.1^b	0	0
实验组	1	1.2±0.1^a	0.8±0.1^a	68±13^a
	30	0.8±0.1^b	0.5±0.1^b	66±10^a
	90	0.7±0.1^b	0.5±0.1^b	69±10^a
	180	0.7±0.1^b	0.5±0.1^b	67±8^a
	270	0.7±0.1^b	0.5±0.1^b	64±8^a

组别	观测时间/d	菌落计数/CFU			乳酸量/mmol·L^-1
组别	观测时间/d	全菌落	总链球菌	变异链球菌	乳酸量/mmol·L^-1
对照组	1	（5.7 ±1.0）×10^{9 a}	（5.9 ±1.1）×10^{8 a}	（6.0 ±1.1）×10^{7 a}	22.5±2.8 ^a
	30	（5.6 ±1.0）×10^{9 a}	（5.8 ±1.0）×10^{8 a}	（6.1 ±1.2）×10^{7 a}	23.7±4.1 ^a
	90	（6.2 ±1.3）×10^{9 a}	（5.6 ±1.0）×10^{8 a}	（5.9 ±1.0）×10^{7 a}	21.6±3.1 ^a
	180	（6.1 ±1.1）×10^{9 a}	（5.7 ±1.0）×10^{8 a}	（6.3 ±1.0）×10^{7 a}	23.1±3.2 ^a
	270	（5.8 ±1.1）×10^{9 a}	（5.9 ±1.2）×10^{8 a}	（6.0 ±1.0）×10^{7 a}	23.9±4.0 ^a
实验组	1	（5.7 ±1.0）×10^{6 b}	（5.7 ±1.0）×10^{5 b}	（5.8 ±1.2）×10^{3 b}	0.23±0.04 ^b
	30	（5.8 ±1.1）×10^{6 b}	（5.6 ±1.0）×10^{5 b}	（6.2 ±1.1）×10^{3 b}	0.22±0.03 ^b
	90	（5.7 ±1.0）×10^{6 b}	（6.0 ±1.0）×10^{5 b}	（6.0 ±1.0）×10^{3 b}	0.26±0.04 ^b
	180	（6.0 ±1.1）×10^{6 b}	（6.1 ±1.1）×10^{5 b}	（6.2 ±1.2）×10^{3 b}	0.25±0.04 ^b
	270	（6.3 ±1.1）×10^{6 b}	（6.1 ±1.2）×10^{5 b}	（6.3 ±1.2）×10^{3 b}	0.24±0.04 ^b

水中浸泡对自修复抗菌复合树脂性能影响的实验研究

Effect of water immersion on a dental self-healing and antibacterial resin composite

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