硅酸盐学报

钛表面电化学沉积氢氧化镁与氧化镁涂层的抗菌性能与生物活性

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杜佳恒 ¹^,² , 范鑫丽 ³ , 肖东琴 ² , 刘刚利 ³ , 尹一然 ¹ , 贺葵 ¹ , 闫吉元 ¹ , 李忠 ¹ , 谭言飞 ⁴ , 段可 ¹

硅酸盐学报 | 研究论文 2024,52(5): 1570-1577

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硅酸盐学报 |研究论文 2024 , 52 (5) : 1570 -1577

钛表面电化学沉积氢氧化镁与氧化镁涂层的抗菌性能与生物活性

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杜佳恒¹^,², 范鑫丽³, 肖东琴², 刘刚利³, 尹一然¹, 贺葵¹, 闫吉元¹, 李忠¹, 谭言飞⁴, 段可¹

作者信息

^1．西南医科大学附属医院骨与关节外科，四川省骨科置入器械研发及应用技术工程实验室，四川泸州 646000

^2．川北医学院第二临床学院，南充市中心医院组织工程与干细胞研究所，四川南充 637000

^3．山东大学齐鲁医学院口腔医学院，口腔医院口腔颌面外科，山东省口腔组织再生重点实验室，山东省口腔生物材料与组织再生工程实验室，山东省口腔疾病临床医学研究中心，济南 250012

^4．四川大学，生物材料工程研究中心，成都 610065

通讯作者:

肖东琴（1986—），女，博士，副研究员；

段可（1973—），男，博士，教授。

作者简介:

杜佳恒（1997—），男，硕士研究生。

Antibacterial Properties and Biological Activities of Magnesium Hydroxide and Magnesium Oxide Coatings by Electrochemical Deposition on Titanium Surface

Jiaheng DU¹^,², Xinli FAN³, Dongqin XIAO², GangLi LIU³, Yiran Yin¹, Kui He¹, Jiyuan Yan¹, Zhong LI¹, Yanfei TAN⁴, Ke DUAN¹

Affiliations

^1.Department of Bone and Joint Surgery, Affiliated Hospital of Southwest Medical University, Sichuan Engineering Laboratory of Orthopaedic Implant R&D and Application Technology, Luzhou 646000, Sichuan, China

^2.Institute of Tissue Engineering and Stem Cell Research, The Second Clinical College of North Sichuan Medical College, Nanchong Central Hospital, Nanchong 637000, Sichuan, China

^3.Department of Oral and Maxillofacial Surgery, School of Stomatology and Hospital of Stomatology, Qilu Medical College, Shandong University, Shandong Key Laboratory of Oral Tissue Regeneration, Shandong Engineering Laboratory of Oral Biomaterials and Tissue Regeneration, Shandong Clinical Medical Research Center of Oral Diseases, Jinan 250012, China

^4.Sichuan University, Biomaterials Engineering Research Center, Chengdu 610065, China

Corresponding Author:

XIAO Dongqin (1986-), female, Ph.D., Associate Professor. E-mail: xiaodongqin@nsmc.edu.cn;

DUAN Ke (1973-), mele, Ph.D., Professor. keduan@swmu.edu.cn

DU Jiaheng (1997-), mele, Master candidate. E-mail: dujiaheng1011@163.com

出版时间: 2024-05-20 doi: 10.14062/j.issn.0454-5648.20230538

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摘要

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骨科植入物相关感染已严重影响手术效果及术后康复，因此需研究具备良好抗菌性能及生物活性的涂层。首先确定电化学沉积氢氧化镁［Mg（OH）₂］及氧化镁（MgO）涂层的制备条件，在钛表面沉积不同时间的Mg（OH）₂及MgO涂层，评价并比较2种涂层的体外抗菌及生物相容性。各组样品表面均匀分布颗粒样物质［Mg（OH）₂及MgO］，颗粒密度与覆盖率随沉积时间增加。Mg（OH）₂及MgO涂层对金黄色葡萄球菌及大肠杆菌均具良好抗菌性且抗菌率随沉积时间增强。沉积≤3 h，MgO抑菌率显著高于Mg（OH）₂；沉积≥6 h，两者抑菌率均接近100%。Mg（OH）₂及MgO涂层细胞毒性随沉积时间上升，其中沉积0.5、1.0 h的2组样品毒性随培养时间下降，其余3组随培养时间上升。沉积0.5 h的Mg（OH）₂及MgO样品与细胞共培养5 d时的细胞存活率为152%、90%；沉积12 h的2组样品与细胞共培养5 d时细胞存活率为2%、6%。研究表明电化学沉积法可成功制备Mg（OH）₂涂层，且煅烧后可获得MgO涂层。沉积1 h的Mg（OH）₂及MgO涂层样品具备良好抗菌性能的同时细胞毒性较小。

关键词

骨科植入物 / 抗菌 / 电化学沉积 / 氢氧化镁 / 氧化镁 / 生物相容性

Abstract

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Introduction

Titanium (Ti)-based implants are one of the most commonly used materials in orthopedic surgery. Although Ti-based implants have good biomechanical properties and biocompatibility, their non-antibacterial shortcomings lead to orthopedic implant-related infections that seriously affect the effect of surgery and postoperative recovery. and serious cases need a second operation and increase the pain and cost of patients. Some studies reported metal or antibiotic antibacterial coatings on Ti-based implants, but they have some disadvantages (i.e., heavy metal coatings can cause damage to the human body, and excessive use of antibiotic coatings can lead to drug resistance). It is thus necessary to investigate the preparation of coatings with good antibacterial properties and biological activities on the surface of Ti-based implants, so as to provide an effective solution to the problem of bone implant-related infection in clinic. Magnesium (Mg) is a major element in human body. Some studies reported that Mg and its compounds have good antibacterial and biocompatibility.

Methods

Ti sheets were cleaned and immersed in an electrolyte containing sodium chloride and magnesium chloride (pH=9.5) and applied a DC voltage of 3.0 V for 0-12 h to obtain magnesium hydroxide [Mg(OH)₂] coatings. After deposition, Mg(OH)₂ coatings were calcined in a muffle furnace at a heating rate of 2 ℃/min at 650 ℃ for 6 h to obtain magnesium oxide (MgO) coatings. The phases of each group of samples were analyzed by X-ray diffraction (XRD), the surface morphology was analyzed by scanning electron microscopy (SEM) and the composition of surface elements was analyzed by energy dispersive spectroscopy (EDS). The in-vitro antibacterial properties of the samples were evaluated according to the standard ISO22196—2011. The bacterial liquid was resuscitated, diluting it to 1 × 10⁵ cfu/mL (cfu is colony-forming units). The samples were firstly sterilized by drying, then 300 μL bacterial solution (i.e., Staphylococcus aureus and Escherichia coli) was then dropped onto each sample and incubated in a constant temperature incubator (at 37 ℃) for 24 h. After diluting the coating plate, the colony number was analyzed and converted to antibacterial rate. The in-vitro cytotoxicity of each sample was evaluated according to the standard ISO10993.5. After dry heat sterilization, the samples were placed in a 24-well plate (no sample cell suspension in the control group and complete culture medium in the blank group). 1mL mouse osteoblast suspensions (OB-6; 5 000 cell/mL) were dropped onto each sample and then incubated in a cell culture box (5% CO₂ at 37 ℃) for 1 d, 3 d or 5 d. After the completion of culture, the absorbance value was detected by a method named CCK-8 and converted to a cell survival rate.

Results and discussion

Mg(OH)₂ coating was prepared on titanium surface by an electrochemical deposition method, and MgO coating was obtained after calcination. Granular matter [Mg(OH)₂ and MgO] are uniformly distributed on the surface of each group, and the particle density and coverage rate increase with deposition time. Mg(OH)₂ and MgO coatings all have a good antibacterial activity against Staphylococcus aureus and Escherichia coli. The antibacterial rates increase with deposition time. When deposited for≤3 h, the antibacterial rate of MgO is higher than that of Mg(OH)₂. After deposited for ≥6 h, the bacteriostatic rate of both is close to 100%. The cytotoxicity of Mg(OH)₂ and MgO coatings increases with the deposition time, and the toxicity of the two groups (i.e., deposited for 0.5 h and 1.0 h) decreases with the culture time, and the toxicity of the other three groups (i.e., deposited for 3 h, 6 h and 12 h) increases with the culture time. At 5 d, the survival rates of Mg(OH)₂ and MgO samples deposited for 0.5 h are 152% and 90%, and the survival rates of the two groups of samples deposited for 12 h are 2% and 6%, respectively.

Conclusions

The surface morphology and thickness of Mg(OH)₂ and MgO coatings changed with the deposition time. The cytotoxicity and antibacterial rate of the coatings were enhanced with the deposition time. It was speculated that there was a dose-effect relationship between them and the coating. The results showed that Mg(OH)₂ coating could be prepared by electrochemical deposition, and the MgO coating could be obtained after calcination. Mg(OH)₂ and MgO coatings deposited for 1 h had good comprehensive properties.

Key words

orthopedic implants / antibacterial / electrochemical deposition / magnesium hydroxide / magnesium oxide / biocompatibility

引用本文

杜佳恒, 范鑫丽, 肖东琴, 刘刚利, 尹一然, 贺葵, 闫吉元, 李忠, 谭言飞, 段可. 钛表面电化学沉积氢氧化镁与氧化镁涂层的抗菌性能与生物活性. 硅酸盐学报, 2024 , 52 (5) : 1570 -1577 . DOI: 10.14062/j.issn.0454-5648.20230538

Jiaheng DU, Xinli FAN, Dongqin XIAO, GangLi LIU, Yiran Yin, Kui He, Jiyuan Yan, Zhong LI, Yanfei TAN, Ke DUAN. Antibacterial Properties and Biological Activities of Magnesium Hydroxide and Magnesium Oxide Coatings by Electrochemical Deposition on Titanium Surface[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (5) : 1570 -1577 . DOI: 10.14062/j.issn.0454-5648.20230538

基金

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四川省科技计划(2020YFS0455; 2022YFS0628)
泸州市-西南医科大学合作项目(2020LZXNYDZ08; 2020LZXNYD F02)
西南医科大学产学研项目(2022CXY03)
泸县西南医科大学联合课题(2020LXXNYKD-01)

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2024年第52卷第5期

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文章信息

doi: 10.14062/j.issn.0454-5648.20230538

接收时间：2023-07-25
首发时间：2026-10-22
出版时间：2024-05-20

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出版历史

收稿日期：2023-07-25
修回日期：2023-09-05

基金

四川省科技计划(2020YFS0455; 2022YFS0628)

泸州市-西南医科大学合作项目(2020LZXNYDZ08; 2020LZXNYD F02)

西南医科大学产学研项目(2022CXY03)

泸县西南医科大学联合课题(2020LXXNYKD-01)

作者信息

^1．西南医科大学附属医院骨与关节外科，四川省骨科置入器械研发及应用技术工程实验室，四川泸州 646000

^2．川北医学院第二临床学院，南充市中心医院组织工程与干细胞研究所，四川南充 637000

^4．四川大学，生物材料工程研究中心，成都 610065

通讯作者:

肖东琴（1986—），女，博士，副研究员；

段可（1973—），男，博士，教授。

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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