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基于生物活性两亲性树莓状纳米颗粒的生物矿化牙本质粘结底漆的制备与表征

Preparation and characterization of biomineralizing dentin bonding primer based on bioactive amphiphilic raspberry-like nanoparticles.

作者信息

Li Qiuju, Huang Guibin, An Wei, Li Ailing, Huang Xiaofeng

机构信息

Department of Stomatology, Beijing Friendship Hospital, Capital Medical University, 95 Yong an Road, Xicheng District, Beijing, 100050, China.

Department of Cariology and Endodontology II, Xiamen Key Laboratory of Stomatological Disease Diagnosis and Treatment, Stomatological Hospital of Xiamen Medical College, Xiamen, China.

出版信息

BMC Oral Health. 2025 Aug 12;25(1):1321. doi: 10.1186/s12903-025-06698-5.

DOI:10.1186/s12903-025-06698-5
PMID:40797203
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC12344852/
Abstract

BACKGROUND

Incomplete resin coverage of demineralized collagen can compromise dentin bond durability. This study developed a biomineralizing dentin bonding primer incorporating bioactive amphiphilic raspberry-like nanoparticles (BRPs) to enhance biomineralization and dentin bond strength.

METHODS

BRPs were characterized using scanning electron microscopy (SEM) and nitrogen (N) adsorption experiments. The ions release from BRPs was measured using inductively coupled plasma mass spectrometry (ICP-MS), while the mineralization was evaluated using SEM and X-ray diffraction (XRD). Subsequently, an etch-and-rinse bonding system was prepared, with primer containing 1%, 5%, or 10% BRPs (w/w). XRD and SEM assessed the biomineralization of each primer group after one-month immersion in simulated body fluid (SBF). Then, 48 dentin plane samples were prepared from extracted non-carious human third molars and bonded with each primer. Stick-shaped samples (n = 30 for each group) were fabricated to evaluate the micro-tensile bond strength (µTBS) after 24 h and 6 months of aging. Degree of conversion (DC) was analyzed via attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR).

RESULTS

BRPs (~ 100 nm) released Ca and SiO in SBF, with surface areas of 83.19 ± 0.52 m/g. After SBF immersion, SEM detected the formation of mineral clusters on BRPs, and XRD analysis confirmed the presence of distinct characteristic peaks corresponding to hydroxyapatite (HAP). Regarding the mineralization of primers, only 5% BRPs-Primer and 10% BRPs-Primer formed needle-like mineral clusters, with distinct HAP characteristic peaks. For the 24-h µTBS, the 1% and 5% BRPs-Primers were comparable to Control-Primer (P > 0.05), but 10% BRPs-Primer showed a significant reduction (P < 0.05). After 6-month aging, 5% BRPs-Primer maintained µTBS compared to its respective 24-h measurements (P > 0.05), whereas µTBS significantly declined in both Control-Primer and 1% BRPs-Primer (P < 0.05). The 5% BRPs-Primer also exhibited a comparable DC to the Control-Primer (P > 0.05), and showed good nanoparticle dispersion and effective penetration into dentinal tubules.

CONCLUSION

BRPs demonstrated superior mineralization ability. Incorporating 5% BRPs into dentin primer achieved effective biomineralization, excellent initial bond strength, and long-term bond stability after 6-month aging.

摘要

背景

脱矿质胶原蛋白的树脂覆盖不完全会损害牙本质粘结耐久性。本研究开发了一种生物矿化牙本质粘结底漆,其包含具有生物活性的两亲性树莓状纳米颗粒(BRP),以增强生物矿化和牙本质粘结强度。

方法

使用扫描电子显微镜(SEM)和氮(N)吸附实验对BRP进行表征。使用电感耦合等离子体质谱(ICP-MS)测量BRP释放的离子,同时使用SEM和X射线衍射(XRD)评估矿化情况。随后,制备一种酸蚀冲洗粘结系统,底漆中含有1%、5%或10%的BRP(重量/重量)。XRD和SEM评估了每个底漆组在模拟体液(SBF)中浸泡一个月后的生物矿化情况。然后,从拔除的无龋人类第三磨牙制备48个牙本质平面样本,并用每种底漆进行粘结。制作棒状样本(每组n = 30)以评估老化24小时和6个月后的微拉伸粘结强度(µTBS)。通过衰减全反射傅里叶变换红外光谱(ATR-FTIR)分析转化率(DC)。

结果

BRP(约100纳米)在SBF中释放钙和硅,表面积为83.19±0.52平方米/克。在SBF浸泡后,SEM检测到BRP上形成矿物簇,XRD分析证实存在对应于羟基磷灰石(HAP)的明显特征峰。关于底漆的矿化,只有5% BRP-底漆和10% BRP-底漆形成针状矿物簇,具有明显的HAP特征峰。对于24小时的µTBS,1%和5% BRP-底漆与对照底漆相当(P > 0.05),但10% BRP-底漆显示出显著降低(P < 0.05)。老化6个月后,5% BRP-底漆与其各自的24小时测量值相比保持了µTBS(P > 0.05),而对照底漆和1% BRP-底漆中的µTBS均显著下降(P < 0.05)。5% BRP-底漆还表现出与对照底漆相当的DC(P > 0.05),并显示出良好的纳米颗粒分散性和有效渗透到牙本质小管中。

结论

BRP表现出卓越的矿化能力。在牙本质底漆中加入5%的BRP可实现有效的生物矿化、优异的初始粘结强度以及老化6个月后的长期粘结稳定性。

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