微纳米生物活性玻璃诱导牙本质再矿化研究

doi:10.15541/jim20210158

无机材料学报 ›› 2022, Vol. 37 ›› Issue (4): 436-444.DOI: 10.15541/jim20210158

微纳米生物活性玻璃诱导牙本质再矿化研究

唐洁吟¹^,²(), 王刚³^,⁴, 刘聪¹^,², 邹学农³^,⁴, 陈晓峰¹^,²()

1.华南理工大学材料科学与工程学院, 生物医学工程系, 广州 510641
2.国家人体组织功能重建工程技术研究中心, 广州 510006
3.中山大学附属第一医院脊柱外科, 广州 510008
4.广东省骨科学重点实验室, 广州 510008

收稿日期:2021-03-12 修回日期:2021-04-08 出版日期:2022-04-20 网络出版日期:2021-04-30
通讯作者: 陈晓峰, 教授. E-mail: chenxf@scut.edu.cn
作者简介:唐洁吟(1989-), 女, 硕士. E-mail: 1720175343@qq.com
基金资助:
国家自然科学基金(52003302);国家自然科学基金(51402108);国家自然科学基金(32071341)

Dentin Remineralization Induced by Micro-nano Bioactive Glass Spheres

TANG Jieyin¹^,²(), WANG Gang³^,⁴, LIU Cong¹^,², ZOU Xuenong³^,⁴, CHEN Xiaofeng¹^,²()

1. Department of Biomedical Engineering, School of Materials Science and Engineering, South China University of Technology, Guangzhou 510641, China
2. National Engineering Research Center for Tissue Restoration and Reconstruction, Guangzhou 510006, China
3. Department of Spine Surgery, The First Affiliated Hospital of Sun Yat-sen University, Guangzhou 510080, China
4. Guangdong Provincial Key Laboratory of Orthopaedics and Traumatology, Guangzhou 510080, China

Received:2021-03-12 Revised:2021-04-08 Published:2022-04-20 Online:2021-04-30
Contact: CHEN Xiaofeng, professor. E-mail: chenxf@scut.edu.cn
About author:TANG Jieyin (1989-), female, Master. E-mail: 1720175343@qq.com
Supported by:
National Natural Science Foundation of China(52003302);National Natural Science Foundation of China(51402108);National Natural Science Foundation of China(32071341)

摘要/Abstract

摘要：

封闭牙本质小管能有效减轻牙齿过敏症。本研究以不同粒径的微纳米生物活性玻璃球(MNBGs)为分散质、海藻酸钠-磷酸盐缓冲溶液为分散液, 制备了用于牙本质脱敏治疗的MNBGs糊剂(MNBGP)。在牙本质切片表面进行体外矿化并系统评价了糊剂与牙本质的结合性能, 以及糊剂体外诱导牙本质再矿化、封闭牙本质小管的能力。研究结果表明, 不同粒径MNBGs制备的糊剂均能与牙本质界面紧密结合, 粒径较小的MNBGs在脱矿牙本质切片表面分布更加均匀。MNBGP在人工唾液(AS)中能较好地诱导牙本质再矿化形成磷灰石(HA)以堵塞封闭牙本质小管, 脱矿牙本质切片表面形成的HA 层随矿化时间延长而增厚, 矿化28 d HA层的厚度可达到5~10 μm。MNBGs的尺寸影响其诱导牙本质再矿化的效果, 当颗粒大小与牙本质小管直径匹配时, MNBGs可以更好地封闭牙本质小管。因此, MNBGP具有良好的治疗牙本质过敏的应用前景。

关键词: 牙本质过敏, 微纳米生物活性玻璃, 磷灰石

Abstract:

Occlusion of dentine tubules may reduce or eliminate dentin hypersensitivity. Here, micro-nano bioactive glass spheres (MNBGs) with various sizes and sodium alginate-phosphate buffer solution were used to prepare bioactive glass pastes (MNBGP) for dentin desensitization. Through mineralization on the surface of dentin samples in vitro, the bonding ability of different pastes with dentin, as well as the ability to induce dentin remineralization and occlude dentin tubules in vitro, was investigated. The results indicated that the MNBGP could be tightly combined with the dentin interface, and the MNBGs with smaller particle sizes were more uniformly distributed on the surface of the demineralized dentin slices. MNBGP could well mineralize in artificial saliva (AS) to form apatite (HA), induce dentin remineralization, and occlude dentin tubules, which resulted in thickening HA layer, formed on the surface of demineralized dentin slices, increased with the prolonged mineralization time, up to 5-10 μm after 28 d dentin remineralization. The size of bioactive glass microspheres had a certain impact on its ability to induce remineralization. When the particle size was equal to the diameter of the exposed dentin tubules, it could better occlude the dentin tubules. All data indicate that MNBGP has potential application for dentin hypersensitivity treatment.

Key words: dentine hypersensitivity, micro-nano bioactive glass spheres, apatite

中图分类号:

TQ174

唐洁吟, 王刚, 刘聪, 邹学农, 陈晓峰. 微纳米生物活性玻璃诱导牙本质再矿化研究[J]. 无机材料学报, 2022, 37(4): 436-444.

TANG Jieyin, WANG Gang, LIU Cong, ZOU Xuenong, CHEN Xiaofeng. Dentin Remineralization Induced by Micro-nano Bioactive Glass Spheres[J]. Journal of Inorganic Materials, 2022, 37(4): 436-444.

图/表 12

表1 不同粒径MNBGs的理论、实际化学组分和试剂用量

Table 1 Theoretical and measured chemical composition, reagent dosage of MNBGs with different particle sizes

Sample	SiO₂ : CaO : P₂O₅(molar ratio)		DDA/g	TEOS/mL
Sample	Theoretical	Measured	DDA/g	TEOS/mL
MNBGs-1	80 : 16 : 4	87.637 : 12.363 : 0	3	8
MNBGs-2		86.289 : 13.696 : 0.015	6	16
MNBGs-3		89.071 : 10.875 : 0.054	6	24

图1 不同粒径的微纳米生物活性玻璃球的SEM(a1~c1)、TEM(a2~c2)照片和粒径分布图(a3~c3)

Fig. 1 SEM (a1-c1), TEM (a2-c2) images and particle size distributions (a3-c3) of MNBGs

图2 三种微纳米生物活性玻璃球的 XRD图谱(a)和FT-IR(b)图谱

Fig. 2 XRD patterns (a) and FT-IR spectra (b) of MNBGs

表2 牙本质切片表面EDTA酸蚀前后各元素含量(摩尔分数)及钙磷比

Table 2 Chemical components (molar percent) and Ca/P ratio on the surface of dentin before and after EDTA etching

Samples	C/%	O/%	Ca/%	P/%	Ca/P
Without etching	0	65.77	20.26	13.97	1.45
With etching	66.82	32.99	0.05	0.14	0.35

图3 牙本质切片样品酸蚀前(a)后(b)的SEM照片(插图为牙本质小管放大照片)及生物活性玻璃糊剂实物照片(c)

Fig. 3 SEM images of the dentin surface without (a) and with (b) EDTA-etching, magnified photo of dentin tubules (insert in (b)), and photo of bioactive glass paste (c)

图4 不同MNBGP涂覆的脱矿牙本质切片表面SEM 照片

Fig. 4 SEM images of demineralized dentin slices coating with different MNBGP (a) MNBGP-1; (b) MNBGP-2; (c) MNBGP-3

图5 脱矿牙本质切片表面涂覆不同MNBGP前后, 以及去离子水冲洗后的全反射-红外光谱

Fig. 5 ATR-FTIR spectra of demineralized dentin surface before and after coating with MNBGP, and after rinsing with water (a) MNBGP-1; (b) MNBGP-2; (c) MNBGP-3

图6 未经材料处理(对照组)(a)和涂覆MNBGP-1(b)、MNBGP-2(c)、MNBGP-3(d)的脱矿牙本质切片在人工唾液中浸泡1 d (a1~d1)、7 d (a2~d2)、14 d (a3~d3)和28 d (a4~d4)后的表面SEM照片

Fig. 6 SEM images of the surfaces of demineralized dentin slices without (a) (control) and with treatment by MNBGP-1 (b), MNBGP-2 (c), and MNBGP-3 (d) after soaking in AS for 1 d (a1-d1), 7 d (a2-d2), 14 d (a3-d3) and 28 d (a4-d4)

图7 未经材料处理(a)和涂覆MNBGP-1(b)、MNBGP-2(c)、MNBGP-3(d)的脱矿牙本质切片在人工唾液中浸泡1 d (a1~d1)、7 d (a2~d2)、14 d (a3~d3)和28 d (a4~d4)后的纵截面的SEM照片

Fig. 7 SEM images of the longitudinal section of demineralized dentin samples without (a) (control) and with treatment by MNBGP-1 (b), MNBGP-2 (c), and MNBGP-3 (d) after soaking in AS for 1 d (a1-d1), 7 d (a2-d2), 14 d (a3-d3) and 28 d (a4-d4)

图8 对照组(a)和MNBGP-1(b)、MNBGP-2(c)、MNBGP-3(d)涂覆的脱矿牙本质切片在人工唾液中矿化28 d表面的EDS能谱分析

Fig. 8 EDS analyses of the surface of demineralized dentin slices without (a) (control) and with treatment by MNBGP-1 (b), MNBGP-2 (c), and MNBGP-3 (d) after soaking in AS for 28 d

表3 脱矿牙本质切片表面钙、磷元素含量(摩尔分数)及钙磷比

Table 3 Chemical components ( molar percent) and Ca/P ratio in molar on the surface of remineralized dentin

Sample	Ca/%	P/%	Ca/P
Control	2.49	1.82	1.37
MNBGP-1	16.64	11.69	1.42
MNBGP-2	18.37	12.97	1.42
MNBGP-3	6.16	6.12	1.01

图9 天然牙本质、脱矿牙本质和在人工唾液中浸泡28 d的脱矿牙本质切片样品表面的XRD 图谱

Fig. 9 XRD patterns of the surface of intact dentin, demineralized dentin and slices without treatment (control) and being treated with MNBGP after being soaked in AS for 28 d

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微纳米生物活性玻璃诱导牙本质再矿化研究

Dentin Remineralization Induced by Micro-nano Bioactive Glass Spheres

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