氨基酸/羟基磷灰石复合材料的制备与表征及其在酸蚀牛牙釉质体外再矿化中的应用

doi:10.11868/j.issn.1001-4381.2019.000259

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摘要

在不同浓度丝氨酸（Ser），天冬氨酸（Asp）和谷氨酸（Glu）的组合下制备氨基酸/羟基磷灰石（AA/HAP）复合材料。通过红外光谱仪、X射线衍射仪和透射电镜对复合材料进行表征，评估复合材料对酸蚀牛牙釉质体外再矿化的效果。结果表明：氨基酸（AA）会干扰羟基磷灰石（HAP）晶面的生长，使HAP的溶解度增加和晶体结构有序性降低。X射线衍射图及透射电镜图的结果显示，AA对HAP的[100]晶向具有显著的抑制作用，且与不含AA的HAP相比，AA修饰的HAP复合材料具有细化的晶粒尺寸。通过CCK-8法评估了材料的细胞毒性，结果表明AA/HAP复合材料的相对细胞活性优于HAP。场发射扫描电镜图表明不含AA的HAP材料和两组不同浓度AA改性HAP材料均可修复酸蚀牛牙釉质的表面龋损。而在Ser，Asp和Glu均为10 mmol·L^-1条件下制备的AA/HAP可在牛牙釉质的深层再矿化中生成厚度约为22 μm的致密再矿化层，并获得了最佳的表面显微硬度恢复效果。

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	刘继涛
	钏定泽
	杨泽斌
	陈希亮
	颜廷亭
	陈庆华

关键词 ：氨基酸, 羟基磷灰石, 复合材料, 生物相容性, 牙釉质, 再矿化

Abstract：

Amino acids modified hydroxyapatite (AA/HAP) composites were synthesized in the presence of different concentrations of serine (Ser), aspartic acid (Asp) and glutamic acid (Glu). The composites were characterized by Fourier transform infrared spectrometer, X-ray diffractometer (XRD) and transmission electron microscope (TEM), and were evaluated in the in vitro remineralization of acid-etched bovine enamel. The results show that amino acids (AA)can interfere with the growth of HAP crystal plane, resulting in the increase of the solubility and decrease of the ordered structure of the HAP crystals. XRD patterns and TEM analysis show that AA has a significant inhibitory effect on the [100] crystalline direction of HAP.Meanwhile, the HAP composites modified by AA have refined crystalline size when compared with the HAP without AA. The cytotoxicity of the materials was evaluated by CCK-8 assay and the results show that the relative cell activity of AA/HAP composites is better than the HAP. Field emission scanning electron microscope images show that the HAP without amino acids and the HAP modified with two different concentrations of amino acids both can repair the surface lesions of bovine enamel. While only the AA/HAP synthesized in the presence of 10 mmol·L^-1 Ser, Asp and Glu generates a dense remineralization layer with a thickness of approximately 22 μm in the subsurface restoration, and obtains the best surface microhardness recovering.

Key words： amino acid hydroxyapatite composite biocompatibility enamel remineralization

收稿日期: 2019-03-21 出版日期: 2020-03-03

中图分类号:

R318.08

通讯作者: 陈庆华 E-mail: 847501438@qq.com

作者简介: 陈庆华(1962-), 男, 教授, 博士, 博士生导师, 研究方向为生物医用材料, 联系地址:云南省昆明市五华区学府路253号昆明理工大学材料科学与工程学院大楼635(650093), E-mail:847501438@qq.com

引用本文:

刘继涛, 钏定泽, 杨泽斌, 陈希亮, 颜廷亭, 陈庆华. 氨基酸/羟基磷灰石复合材料的制备与表征及其在酸蚀牛牙釉质体外再矿化中的应用[J]. 材料工程, 2020, 48(2): 100-107.
Ji-tao LIU, Ding-ze CHUAN, Ze-bin YANG, Xi-liang CHEN, Ting-ting YAN, Qing-hua CHEN. Synthesis and characterization of amino acids/hydroxyapatite composites for in vitro remi-neralization of acid-etched bovine enamel. Journal of Materials Engineering, 2020, 48(2): 100-107.

链接本文:

http://jme.biam.ac.cn/CN/10.11868/j.issn.1001-4381.2019.000259 或 http://jme.biam.ac.cn/CN/Y2020/V48/I2/100

Table 1 Ser，Asp和Glu的浓度

Fig.1 HAP-0，HAP-5和HAP-10的FTIR图

Fig.2 HAP-0，HAP-5和HAP-10的XRD图

Table 2 根据XRD数据计算的晶粒尺寸

Fig.3 再矿化溶液上清液中Ca²⁺浓度

Fig.4 复合材料的TEM(1)与HRTEM(2)图
(a)HAP-0；(b)HAP-5；(c)HAP-10

Fig.5 复合材料对细胞相对活性的影响

Fig.6 牙釉质表面(1)和剖面(2)FESEM图
(a)抛光牙釉质；(b)酸蚀牙釉质

Fig.7 再矿化后牙釉质表面(1)和剖面(2)FESEM图
(a)空白组；(b)HAP-0；(c)HAP-5；(d)HAP-10

Fig.8 再矿化前后SMH值对比图

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