Dental Materials最新文献_第2页

Long-term effect of ammonia- and water-based silver fluoride on dentin collagen matrix 氨和水基氟化银对牙本质胶原基质的长期影响。

IF 6.3 1区医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE

Dental Materials

Pub Date : 2026-04-01 Epub Date: 2025-11-04 DOI: 10.1016/j.dental.2025.10.016

Merve Uctasli , Roda Seseogullari-Dirihan , Thiago Henrique Scarabello Stape , Mustafa Murat Mutluay , Arzu Tezvergil-Mutluay

Objective

To evaluate the long-term effect of ammonia- and water-based silver fluoride treatments on the degradation of the dentin collagen matrix.

Methods

Dentin beams (0.3x3x7mm) were demineralized (10 % H₃PO₄), rinsed and randomly distributed into six groups. Groups (n = 10 beams/group) were treated with (1) ammonia-based silver fluoride = SDF; (2) SDF + potassium iodide = KI (3) water-based silver fluoride = SF (4) SF + KI (5) KI (6) untreated demineralized dentin beams served as control. Following treatments, dry mass, modulus of elasticity and enzymatic activity were assessed. Dentin beams were incubated in calcium- and zinc-containing artificial saliva up to 6 months. After different incubation periods (1 week, 1 month, 3 months or 6 months), dry mass, modulus of elasticity and enzymatic activity were reevaluated. The aliquots of incubation media were analyzed to determine the solubilized telopeptides of collagen (ICTP and CTX immunoassays), hydroxyproline release and total extractable protein (Bradford assay). Scanning electron microscopy imaging and in situ zymography analyses were conducted. Data were statistically analyzed with ANOVA followed by Tukey test (α=0.05).

Results

Silver fluoride treatments reduced the total enzymatic activity, but increased the solubilized telopeptides of collagen throughout incubation periods (p < 0.05). The addition of KI exacerbated the loss of dry mass, modulus of elasticity, hydroxyproline release and total protein loss (p < 0.05).

Significance

Ammonia- and water-based silver fluoride treatments may reduce long-term degradation of dentin collagen. However, potassium iodide can further increase endogenous protease activity and compromise the structural integrity of dentin’s organic matrix.

目的：评价氨基氟化银和水基氟化银对牙本质胶原基质降解的远期影响。方法：牙本质梁（0.3x3x7mm）脱矿（10 % H3PO4），冲洗后随机分为6组。各组（n = 10束/组）用(1)氨基氟化银= SDF处理；(2) SDF + 碘化钾= KI(3)水基氟化银= SF (4) SF + KI (5) KI(6)未处理脱矿牙本质光束作为对照。处理后，测定其干质量、弹性模量和酶活性。牙本质梁在含钙和含锌的人工唾液中孵育6个月。在不同的孵育期（1周、1个月、3个月或6个月）后，重新评估干质量、弹性模量和酶活性。分析培养液的等分，以测定胶原蛋白的溶解端肽（ICTP和CTX免疫测定）、羟脯氨酸释放量和总可提取蛋白（Bradford测定）。扫描电镜成像和原位酶谱分析。资料采用方差分析和Tukey检验（α=0.05）进行统计学分析。结果：氟化银处理降低了总酶活性，但在整个孵育期间增加了胶原的可溶性端肽（p ）。意义：氨和水基氟化银处理可能会减少牙本质胶原的长期降解。然而，碘化钾会进一步增加内源性蛋白酶的活性，损害牙本质有机基质的结构完整性。

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引用次数: 0

A novel method to assess the interfacial fracture toughness of two universal resin cements to dentin 一种评估两种通用树脂黏合剂与牙本质界面断裂韧性的新方法。

IF 6.3 1区医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE

Dental Materials

Pub Date : 2026-04-01 Epub Date: 2025-12-13 DOI: 10.1016/j.dental.2025.12.004

Tony Lorey , Jennifer Woolford , Markus B. Blatz , Ulrich Lohbauer , Renan Belli , José Ignacio Zorzin

Objective

The purpose of this study was to evaluate the adhesion potential of two universal resin cements compared to a gold standard adhesive system, considering application mode and storage time, using a novel method for interfacial fracture toughness (iFT).

Methods

iFT was measured using the Chevron-Notched Beam (CNB) method with a novel modified split-CNB sandwich specimen design. One hundred human third molars were sectioned into enamel-dentin rods, adhesively conditioned, notched, and cut apart in the dentin area. Specimens were bonded using the universal luting resin in self-adhesive mode or with their corresponding adhesive system/primer (RelyX Universal and Scotchbond Universal Plus, Solventum; GCem One and Adhesive Enhancing Primer, GC Corp.). A gold standard adhesive (OptiBond FL, Kerr) in combination with a flowable resin composite as luting material (x-tra base Universal, VOCO) served as a control. The influence of storage time (24 h vs. 180 days), application mode (adhesive vs. self-adhesive), and the material itself on the iFT measured as fracture toughness in mode I (K_Ic) according to ASTM C1421–10 was evaluated. Scanning electron microscopy (SEM) was employed to analyze interfacial characteristics and failure modes.

Results

Statistical analysis (Kruskal-Wallis H test with Bonferroni-Holm correction) revealed significant differences in iFT between the groups. Specimens stored for 180 days exhibited lower iFT compared to those stored for 24 h. The adhesive application significantly enhanced iFT relative to the self-adhesive mode. GCem One with Adhesive Enhancing Primer (24 h) exhibited the highest interfacial fracture toughness among all investigated groups. SEM analysis indicated a predominance of adhesive failures at the dentin-resin interface, particularly within the self-adhesive groups.

Conclusions

The application mode and material significantly influence interfacial fracture toughness. The adhesive-assisted application enhances bond stability, while the self-adhesive approach exhibits lower long-term adhesion.

Clinical significance

The use of universal resin cements along with their adhesive system/primer significantly enhances adhesion between the tooth and the restoration, leading to improved long-term clinical success. For restorations without microretention, universal resin cements must be used in combination with their adhesive system/primer.

目的：本研究的目的是利用一种新的界面断裂韧性（iFT）方法，在考虑应用方式和储存时间的情况下，比较两种通用树脂胶合剂与金标准胶粘剂体系的粘合潜力。方法:使用Chevron-Notched界面张力测量光束(CNB)方法与小说split-CNB三明治标本设计修改。将100颗人第三磨牙切成牙釉质-牙本质棒，在牙本质区域进行粘合、切槽和切割。标本使用通用粘接树脂以不干胶模式粘合或使用相应的粘合系统/底漆（RelyX universal和Scotchbond universal Plus， Solventum； GCem One和adhesive enhanced primer， GC Corp.）粘合。金标准粘合剂（OptiBond FL, Kerr）与可流动树脂复合材料（x-tra base Universal， VOCO）结合作为对照。根据ASTM C1421-10评估了储存时间（24 h vs 180天）、应用方式（粘合剂vs.不粘胶）和材料本身对I模式断裂韧性（KIc）测量的iFT的影响。采用扫描电镜（SEM）对界面特征和失效模式进行了分析。结果：统计学分析（Kruskal-Wallis H检验和Bonferroni-Holm校正）显示两组间iFT有显著差异。与保存24 h的标本相比，保存180天的标本显示出较低的iFT。相对于不干胶模式，胶粘剂的应用显著增强了iFT。GCem 1与粘合剂增强底漆（24 h）表现出最高的界面断裂韧性。扫描电镜分析表明，牙本质-树脂界面的粘合失效占主导地位，特别是在自粘合组中。结论：应用方式和材料对界面断裂韧性有显著影响。粘合剂辅助应用增强了粘合稳定性，而不干胶方法表现出较低的长期附着力。临床意义：通用树脂骨水泥及其粘接系统/底物的使用显著增强了牙齿与修复体之间的粘连性，提高了长期的临床成功率。对于没有微固位的修复体，通用树脂胶合剂必须与粘合剂系统/底漆结合使用。

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引用次数: 0

Fluorine plasma etching modulates submicron topography, physico-chemical aging and biological responses of titanium dental implants 氟等离子体刻蚀对钛牙种植体亚微米形貌、物理化学老化和生物反应的影响。

IF 6.3 1区医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE

Dental Materials

Pub Date : 2026-04-01 Epub Date: 2025-12-17 DOI: 10.1016/j.dental.2025.12.006

Frank Rupp , Barbara Illing , Nadja Felde , Zeqian Xu , Jacob Schultheiss , Evi Kimmerle-Müller , Leila Mohammadnejad , Stefanie Krajewski

Objectives

Surface topography, surface chemistry, as well as wetting properties of dental titanium implants are decisive parameteres that modulate biological responses. Problems arise when the optimal wetting properties of as-fabricated implants are compromised by aging effects due to renewed contamination and renewed hydrophobization during storage.

The primary objective of this study is to investigate the effects of plasma etching on titanium using fluorine-containing gases, focusing on submicron and nano-scale topographical changes, long-term wetting characteristics, hydrocarbon contaminations, and cellular and bacterial responses.

Methods

Machined titanium reference samples (M) were either plasma-treated by reactive ion etching with CF₄ and NF₃ gases (MCF4, MNF3), or modified by a superimposed nanotopography (Mnano). All samples were hydrophilized by O₂-plasma (new variants), further processed by 14 d storage (aged variants), and were characterized by FE-SEM, AFM, EDX, XPS, and contact angle analyses. Biological experiments were performed in vitro to evaluate possible effects of the prepared surfaces on soft and hard tissue cells by focal contact analysis, CCK8, and alizarin red staining, as well as on bacterial adhesion by crystal violet staining.

Results

CF₄ and NF₃ plasma treatments generated a tight network of submicron pores. MNF3 showed distinct physico-chemical non-aging properties with long-lasting hydrophilicity. The new surface of MNF3 significantly reduced the adhesion of Streptococcus gordonii. However, neither MCF4 nor MNF3 significantly improved the cellular response. In contrast, the highest number of HGF focal contacts indicating improved soft tissue attachment was observed on aged M and Mnano surfaces. Furthermore, HGF metabolic activity declined on new MCF4 and MNF3, compared to M and Mnano.

Significance

This study shows promising antibacterial potential of the new NF₃ plasma-etched titanium implant surface modification. However, this study also indicates that machined surfaces, due to their already promising soft tissue cellular responses, cannot simply be surpassed by novel fluorine plasma etched surface modifications. Therefore, a zonal arrangement of the transmucosal portion of implant and abutment areas with basal sealing and coronal antibacterial functionalities is suggested.

目的：牙钛种植体的表面形貌、表面化学和湿润特性是调节生物反应的决定性参数。当制备的植入物的最佳润湿性能受到老化效应的影响时，由于在储存过程中重新污染和重新疏水性，问题就出现了。本研究的主要目的是研究含氟气体等离子体蚀刻对钛的影响，重点关注亚微米和纳米尺度的地形变化、长期润湿特性、碳氢化合物污染以及细胞和细菌的反应。方法：用CF4和NF3气体（MCF4, MNF3）反应离子刻蚀等离子体处理加工后的钛参考样品(M)，或用叠加纳米形貌（Mnano）修饰。所有样品都经过o2等离子体（新变体）的亲水性处理，经过14 d的储存处理（老化变体），并通过FE-SEM， AFM， EDX， XPS和接触角分析进行了表征。体外生物实验通过局灶接触分析、CCK8和茜素红染色评价制备的表面对软硬组织细胞的可能影响，结晶紫染色评价制备的表面对细菌粘附的可能影响。结果：CF4和NF3等离子体处理产生了紧密的亚微米孔网络。MNF3具有明显的物理化学不老化性能和持久的亲水性。MNF3的新表面明显降低了gordonii链球菌的粘附。然而，MCF4和MNF3均未显著改善细胞应答。相比之下，在老化的M和Mnano表面上观察到的HGF焦点接触数量最多，表明软组织附着改善。此外，与M和Mnano相比，HGF在新MCF4和MNF3上的代谢活性下降。意义：本研究显示新型NF3等离子蚀刻钛种植体表面改性具有良好的抗菌潜力。然而，这项研究还表明，由于其已经有希望的软组织细胞反应，加工表面不能简单地被新型氟等离子体蚀刻表面修饰所超越。因此，建议种植体的跨粘膜部分和基牙区域的带状排列具有基底密封和冠状抗菌功能。

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引用次数: 0

Cytotoxicity testing of dental materials: Establishment of a 3D-printed dentin barrier culture system 牙科材料的细胞毒性测试：3d打印牙本质屏障培养系统的建立。

IF 6.3 1区医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE

Dental Materials

Pub Date : 2026-04-01 Epub Date: 2025-12-02 DOI: 10.1016/j.dental.2025.11.016

Ella Ohlsson , Sandra Pohl , Iryna Prots , Carola Bolay , Kerstin M. Galler , Wolfgang Buchalla , Gottfried Schmalz , Matthias Widbiller

Introduction

Cytotoxicity testing is critical in assessing the biocompatibility of dental materials with regard to the pulp, however, conventional methods such as the extract test (ISO 10993–5) do not reflect the protective effects of dentin in the dentin-pulp complex. Traditional dentin barrier testing techniques (ISO 7405) address this problem, but face challenges due to their complex and expensive production and the difficult and error-prone handling. Therefore, the aim of this study was to develop a novel, user-friendly and easily accessible dentin barrier culture system (DBCS) to improve cytotoxicity testing of dental materials.

Method

The DBCS was designed and manufactured using stereolithography 3D printing. The components were assembled with dentin discs to create a barrier between an upper and lower compartment (pulp side/restoration side). Dentin discs were pretreated (EDTA or citric acid) and primary human pulp cells (HPC) or mouse fibroblasts (L-929) were cultured in the upper chamber, while a self-adhesive composite (Vertise Flow, Kerr; Scafati, Italy) was applied to the opposite side of the disc after 48 h. Scanning electron microscopy (SEM) was used to visualize dentin structure and cell attachment. Analyses included assessment of cell metabolism (MTT test), membrane integrity (LDH assay), and performing live/dead staining. To validate the model, various dentin disc parameters were evaluated, including species origin (human or bovine), location relative to the pulp (proximal or distal), thickness, and the effects of autoclaving. Statistical evaluation was performed using the Kruskal-Wallis or the Mann-Whitney test (P ≤ 0.05).

Results

Both HPC and L-929 formed confluent cell layers in the DBCS setup. Pretreatment of dentin discs with EDTA or citric acid reliably removed the smear layer, with the latter having a positive effect on cell viability (P ≤ 0.03). The self-adhesive composite had a similar effect on the viability of both cell types, and SEM revealed apoptotic cell morphology. Dentin provided a protection only at a thickness of greater than 400 µm. There were no significant differences in cellular responses to the material depending on dentin origin or autoclaving (P > 0.9999).

Conclusion

This 3D-printable culture system offers a readily available, user-friendly dentin barrier model for evaluating the cytotoxicity of dental materials and can be easily reproduced by anyone with access to a standard 3D printer.

导言：细胞毒性测试是评估牙髓生物相容性的关键，然而，传统的方法，如提取物测试（ISO 10993-5）不能反映牙本质在牙本质-牙髓复合体中的保护作用。传统的牙本质屏障测试技术（ISO 7405）解决了这个问题，但由于其复杂和昂贵的生产以及困难和容易出错的处理，面临着挑战。因此，本研究的目的是开发一种新型的、用户友好的、易于使用的牙本质屏障培养系统（DBCS），以改善牙科材料的细胞毒性检测。方法：采用立体光刻3D打印技术设计制作DBCS。组件与牙本质盘组装，在上下隔室（牙髓侧/修复侧）之间形成屏障。对牙本质盘进行预处理（EDTA或柠檬酸），上腔培养原代人牙髓细胞（HPC）或小鼠成纤维细胞（L-929）， 48 h后将自粘复合材料（Vertise Flow, Kerr; Scafati, Italy）涂于牙本质盘的另侧。扫描电镜观察牙本质结构和细胞附着情况。分析包括评估细胞代谢（MTT试验），膜完整性（LDH测定），并进行活/死染色。为了验证该模型，评估了各种牙本质椎间盘参数，包括物种来源（人类或牛），相对于牙髓的位置（近端或远端），厚度以及高压灭菌的效果。采用Kruskal-Wallis或Mann-Whitney检验进行统计学评价（P ≤ 0.05）。结果：HPC和L-929在DBCS中均形成融合细胞层。EDTA或柠檬酸预处理牙本质盘可靠地去除涂片层，后者对细胞活力有积极影响（P ≤ 0.03）。自粘复合材料对两种细胞的活力有相似的影响，扫描电镜显示凋亡的细胞形态。牙本质仅在厚度大于400 µm时提供保护。根据牙本质来源或高压灭菌，细胞对材料的反应没有显著差异（P > 0.9999）。结论：这种3D打印培养系统提供了一种易于获得的、用户友好的牙本质屏障模型，用于评估牙科材料的细胞毒性，任何人都可以使用标准3D打印机轻松复制。

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引用次数: 0

Dentin bonding agents and camphorquinone-induced cytotoxicity, 8-isoprostane and prostaglandin production is associated with CYP450, NQO1, NQO2, GST, and GSH peroxidase in human dental pulp cells 牙本质结合剂和脑啡酮诱导的细胞毒性、8-异前列腺素和前列腺素的产生与人牙髓细胞中CYP450、NQO1、NQO2、GST和GSH过氧化物酶有关。

IF 6.3 1区医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE

Dental Materials

Pub Date : 2026-04-01 Epub Date: 2025-11-28 DOI: 10.1016/j.dental.2025.11.013

Mei-Chi Chang , Tai-Min Lin , Wan-Chuen Liao , Ju-Hui Wu , Shyuan-Yow Chen , Hsueh-Wei Chang , Wen-Hui Chen , Hsiao-Hua Chang , Jiiang-Huei Jeng

Objective

Camphorquinone (CQ) is a photo-initiator popularly-included in the dentin bonding agent (DBA) and composite resin for tooth decay restoration. CQ application during operative procedures may affect the viability and inflammation of dental pulp. Cytochrome P450 (CYP), NAD(P)H quinone oxidoreductase (NQO) 1 and NQO2, glutathione S-transferase (GST), and glutathione peroxidase (GPx) are crucial enzymes for metabolism of chemicals with quinone structure. The expression and involvement of various enzymes in CQ metabolism and toxicity were investigated. Methods: Human dental pulp cells (HDPCs) were treated by four DBAs or CQ with/without inhibitors (α-naphthoflavone [CYP inhibitor], dicoumarol & ES936 [NQO1 inhibitors] or quercetin or melatonin [NQO2 inhibitors], ethacrynic acid [GST-P inhibitor], a26 [GPx4 inhibitor], cefoxitin [GPx1 inhibitor]) for 24 h. Enzyme-linked immunosorbent assay was used for 8-isoprostane, and PGE₂ analysis in culture medium. MTT assay was used for cell viability estimation. Real-time PCR and immunofluorescent staining were used for mRNA/protein expression analysis. Results: We found that in various concentrations, four clinically-used DBAs induced 8-isoprostane and PGE₂ production in HDPCs. CQ stimulated CYP1A1, CYP1A2, NQO1, NQO2, GST-P, GPx1 and GPx4 mRNA and protein expression, and some of the stimulation can be attenuated by U0126 (a MEK/ERK inhibitor). The α-naphthoflavone, ES936, ethacrynic acid, melatonin and a26 showed little effect on the CQ-induced cytotoxicity to HDPCs. Most inhibitors (α-naphthoflavone, dicoumarol, ES936, quercetin, melatonin, a26) except ethacrynic acid and cefoxitin showed preventive effect on CQ-induced PGE₂ and 8-isoprostane production, but to a different extent.

Significance

DBAs and CQ may affect the inflammatory responses and tissue viability of dental pulp during clinical dental practice. Expression of CYPs, NQO1/NQO2, GST-P and GPx in HDPCs affects the metabolism of CQ, cell viability, 8-isoprostane and PGE₂ of HDPCs. Results are important for the clinical success of operative restoration to decrease pulp inflammation and necrosis by modulation of these metabolic enzymes.

目的：樟脑醌（Camphorquinone， CQ）是一种光引发剂，广泛应用于牙本质粘结剂（DBA）和牙本质修复复合树脂中。在手术过程中使用CQ可能会影响牙髓的活力和炎症。细胞色素P450 （CYP）、NAD(P)H醌氧化还原酶（NQO） 1和NQO2、谷胱甘肽s -转移酶（GST）和谷胱甘肽过氧化物酶（GPx）是醌类化学物质代谢的关键酶。研究了各种酶在CQ代谢和毒性中的表达和参与。方法：人牙髓细胞（HDPCs）分别用4种DBAs或CQ（含/不含抑制剂）（α-萘黄酮[CYP抑制剂]、二oumarol & ES936 [NQO1抑制剂]或槲皮素或褪黑素[NQO2抑制剂]、乙酸[GST-P抑制剂]、a26 [GPx4抑制剂]、头孢西丁[GPx1抑制剂]）处理24 h。8-异前列腺素采用酶联免疫吸附法，培养基中PGE2分析。MTT法测定细胞活力。采用Real-time PCR和免疫荧光染色进行mRNA/protein表达分析。结果：我们发现，在不同浓度下，四种临床使用的dba诱导HDPCs产生8-异前列腺素和PGE2。CQ可刺激CYP1A1、CYP1A2、NQO1、NQO2、GST-P、GPx1和GPx4 mRNA和蛋白的表达，部分刺激可被MEK/ERK抑制剂U0126减弱。α-萘黄酮、ES936、乙酸、褪黑素和a26对cq诱导的HDPCs细胞毒性影响不大。除乙酸和头孢西丁外，大多数抑制剂（α-萘黄酮、二豆豆醇、ES936、槲皮素、褪黑素、a26）对cq诱导的PGE2和8-异前列腺素产生均有预防作用，但程度不同。意义：dba和CQ在临床牙科治疗中可能影响牙髓的炎症反应和组织活力。HDPCs中CYPs、NQO1/NQO2、GST-P和GPx的表达影响HDPCs的CQ代谢、细胞活力、8-异前列腺素和PGE2的表达。通过调节这些代谢酶来减少牙髓炎症和坏死，对手术修复的临床成功具有重要意义。

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引用次数: 0

EDTA functionalized mesoporous silica (mSiO2-EDTA) for Ca2 + and Zn2+ rechargeable dental resin composites EDTA功能化介孔二氧化硅（mSiO2-EDTA）用于Ca2 +和Zn2+可充电牙科树脂复合材料。

IF 6.3 1区医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE

Dental Materials

Pub Date : 2026-04-01 Epub Date: 2025-12-17 DOI: 10.1016/j.dental.2025.12.008

Jiahui Huang , Hongxia Zhang , Xiangyu Zhang , Yueyue Wang

Objective

The aim of this study was to (1) graft ethylenediamine tetraacetic acid (EDTA) onto mesoporous SiO₂ (mSiO₂) fillers to fabricate Ca²⁺ and Zn²⁺ rechargeable dental composites, (2) investigate the effect of EDTA modification on the properties of the composite resins.

Methods

EDTA modified mSiO₂ (mSiO₂-EDTA) were prepared by a facile one-step silylating reaction. Ca²⁺ and Zn²⁺ were adsorbed onto mSiO₂-EDTA via an ion solution immersing method to obtain mSiO₂-EDTA-Ca and mSiO₂-EDTA-Zn. The ion release behavior and recharge ability of the particles was investigated. Different mass fractions (5, 10, and 20 %) of the functional fillers were added into dental resins to investigate the ion release behavior of the composites. Dental composites containing 20 % fillers were selected to assess their ion recharge capacity, the remineralization potential of mSiO₂-EDTA-Ca loaded composites, and the antibacterial efficacy of those incorporating mSiO₂-EDTA-Zn. The effect of the fillers on the mechanical properties, light-curing performance, and biocompatibility of the dental composites was further evaluated.

Results

mSiO₂-EDTA were successfully synthesized, and Ca²⁺ and Zn²⁺ were adsorbed on the particles by the ion solution immersing method. The ions within the mSiO₂-EDTA-Ca and mSiO₂-EDTA-Zn particles as well as their corresponding dental composites could be released at acidic conditions, and fully recharged after releasing. Even after 10 release-recharge cycles, the ions in the dental resins could still be fully recharged by simply immersing the samples in ion solution for just 10 min. The continually released Ca²⁺ and Zn²⁺ exhibited corresponding functions as promoting mineralization or antibacterial activity. Furthermore, surface modification of mSiO₂ with EDTA did not affect the mechanical properties, light curing performance, and biocompatibility of dental composites.

Conclusion

Novel dental composites with fully Ca²⁺ and Zn²⁺ recharge ability were obtained by surface functionalization of mSiO₂ fillers with EDTA, which provided a potential way for the inhibition of secondary caries.

目的：研究乙二胺四乙酸（EDTA）在介孔SiO2 （mSiO2）填料上接枝制备Ca2+和Zn2+可充电牙科复合材料；研究EDTA改性对复合树脂性能的影响。方法：采用一步硅化反应制备EDTA改性mSiO2 （mSiO2-EDTA）。采用离子溶液浸泡法将Ca2+和Zn2+吸附在mSiO2-EDTA上，得到mSiO2-EDTA- ca和mSiO2-EDTA- zn。研究了颗粒的离子释放行为和充电能力。在牙用树脂中加入不同质量分数（5%、10%和20% %）的功能填料，考察复合材料的离子释放行为。选择含有20 %填料的牙科复合材料，评估其离子充电能力，mSiO₂-EDTA-Ca负载复合材料的再矿化潜力，以及含有mSiO₂-EDTA-Zn的复合材料的抗菌效果。进一步评价了填料对口腔复合材料力学性能、光固化性能和生物相容性的影响。结果：成功合成了mSiO2-EDTA，并通过离子溶液浸泡法吸附了Ca2+和Zn2+。mSiO2-EDTA-Ca和mSiO2-EDTA-Zn颗粒内的离子及其相应的牙用复合材料在酸性条件下可以被释放，释放后可以完全充电。即使经过10次释放-充电循环，牙科树脂中的离子仍然可以通过简单地将样品浸泡在离子溶液中10 min来完全充电。持续释放的Ca2+和Zn2+表现出相应的促进矿化或抗菌活性的功能。此外，EDTA对mSiO2的表面改性不会影响牙科复合材料的力学性能、光固化性能和生物相容性。结论：利用EDTA对mSiO2填料进行表面功能化，可获得具有充分Ca2+和Zn2+充电能力的新型牙体复合材料，为抑制继发性龋提供了一种潜在的途径。

{"title":"EDTA functionalized mesoporous silica (mSiO2-EDTA) for Ca2 + and Zn2+ rechargeable dental resin composites","authors":"Jiahui Huang , Hongxia Zhang , Xiangyu Zhang , Yueyue Wang","doi":"10.1016/j.dental.2025.12.008","DOIUrl":"10.1016/j.dental.2025.12.008","url":null,"abstract":"<div><h3>Objective</h3><div>The aim of this study was to (1) graft ethylenediamine tetraacetic acid (EDTA) onto mesoporous SiO<sub>2</sub> (mSiO<sub>2</sub>) fillers to fabricate Ca<sup>2+</sup> and Zn<sup>2+</sup> rechargeable dental composites, (2) investigate the effect of EDTA modification on the properties of the composite resins.</div></div><div><h3>Methods</h3><div>EDTA modified mSiO<sub>2</sub> (mSiO<sub>2</sub>-EDTA) were prepared by a facile one-step silylating reaction. Ca<sup>2+</sup> and Zn<sup>2+</sup> were adsorbed onto mSiO<sub>2</sub>-EDTA via an ion solution immersing method to obtain mSiO<sub>2</sub>-EDTA-Ca and mSiO<sub>2</sub>-EDTA-Zn. The ion release behavior and recharge ability of the particles was investigated. Different mass fractions (5, 10, and 20 %) of the functional fillers were added into dental resins to investigate the ion release behavior of the composites. Dental composites containing 20 % fillers were selected to assess their ion recharge capacity, the remineralization potential of mSiO₂-EDTA-Ca loaded composites, and the antibacterial efficacy of those incorporating mSiO₂-EDTA-Zn. The effect of the fillers on the mechanical properties, light-curing performance, and biocompatibility of the dental composites was further evaluated.</div></div><div><h3>Results</h3><div>mSiO<sub>2</sub>-EDTA were successfully synthesized, and Ca<sup>2+</sup> and Zn<sup>2+</sup> were adsorbed on the particles by the ion solution immersing method. The ions within the mSiO<sub>2</sub>-EDTA-Ca and mSiO<sub>2</sub>-EDTA-Zn particles as well as their corresponding dental composites could be released at acidic conditions, and fully recharged after releasing. Even after 10 release-recharge cycles, the ions in the dental resins could still be fully recharged by simply immersing the samples in ion solution for just 10 min. The continually released Ca<sup>2+</sup> and Zn<sup>2+</sup> exhibited corresponding functions as promoting mineralization or antibacterial activity. Furthermore, surface modification of mSiO<sub>2</sub> with EDTA did not affect the mechanical properties, light curing performance, and biocompatibility of dental composites.</div></div><div><h3>Conclusion</h3><div>Novel dental composites with fully Ca<sup>2+</sup> and Zn<sup>2+</sup> recharge ability were obtained by surface functionalization of mSiO<sub>2</sub> fillers with EDTA, which provided a potential way for the inhibition of secondary caries.</div></div>","PeriodicalId":298,"journal":{"name":"Dental Materials","volume":"42 4","pages":"Pages 670-682"},"PeriodicalIF":6.3,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145779942","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

The effect of microstructural, compositional, and rheology-based properties of universal adhesive systems on bond strength. 通用胶粘剂体系的微观结构、成分和流变性能对粘接强度的影响。

IF 6.3 1区医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE

Dental Materials

Pub Date : 2026-03-20 DOI: 10.1016/j.dental.2026.03.160

Fikri Öcal, Ayşe Karabaş, Buse Çebi Gül

Objective: The aim of this study was to compare the rheological parameters, hybrid layer thicknesses, inorganic filler contents determined by thermogravimetric analysis (TGA), and elemental compositions obtained by energy-dispersive X-ray spectroscopy (EDX) of five different universal adhesives (G-Premio Bond [GPB], Clearfil Universal Bond [CUB], Prime Bond Universal [PBU], OptiBond Universal [OBU], and Gluma Bond Universal [GBU]) and to evaluate the relationship of these parameters with microtensile bond strength.

Materials and methods: Universal adhesives were applied to dentin specimens obtained from human permanent teeth. Rheological properties were measured with an oscillatory rheometer (0.3 mm gap, 2 Hz, 23 °C) in terms of viscosity, storage modulus, and loss modulus. Adhesive layer thicknesses were measured under a scanning electron microscope at × 1000 magnification, inorganic filler ratios were determined by TGA (30-600 °C), and elemental compositions were assessed by EDX. In addition, microtensile bond strength tests were performed, and the obtained values were compared with rheological, morphological, and chemical parameters.

Results: Rheological analysis revealed that CUB exhibited the highest complex viscosity and modulus values, while PBU showed the lowest (p < 0.05). CUB produced the thickest adhesive, whereas PBU had the thinnest. TGA results indicated that OBU had the highest inorganic filler content, and PBU the lowest. Mechanical testing showed that OBU achieved the highest bond strength, while PBU demonstrated the lowest (p < 0.05). Despite showing no significant elemental differences in EDX analysis, GBU, together with GPB, presented the second-highest bond strength.

Clinical significance: Microstructural features, compositional characteristics, and rheology-based properties of universal adhesives are important factors influencing both bond strength and adhesive layer formation, and evaluating these parameters together may contribute to more predictable clinical outcomes.

摘要目的:本研究的目的是比较五种不同的通用胶粘剂（G-Premio Bond [GPB]、Clearfil universal Bond [CUB]、Prime Bond universal [PBU]、OptiBond universal [OBU]、GPB [GPB]）的流变参数、杂化层厚度、无机填料含量（TGA）和能量色散x射线光谱（EDX）的元素组成。和Gluma Bond Universal [GBU])，并评估这些参数与微拉伸粘结强度的关系。材料与方法：采用万向胶粘剂对恒牙牙本质标本进行粘接。用振荡流变仪（0.3 mm间隙，2 Hz, 23°C）测量粘度、储存模量和损失模量。用扫描电子显微镜（ 1000倍）测量胶粘剂层厚度，用热重分析仪（30-600℃）测定无机填料比例，并用EDX测定元素组成。此外，还进行了微拉伸粘结强度测试，并将所得值与流变学、形态学和化学参数进行了比较。结果：流变学分析显示，CUB具有最高的复合粘度和模量值，而PBU具有最低的复合粘度和模量值（p ）。临床意义：微观结构特征、成分特征和基于流变学的特性是影响粘接强度和粘接层形成的重要因素，综合评估这些参数可能有助于更可预测的临床结果。

{"title":"The effect of microstructural, compositional, and rheology-based properties of universal adhesive systems on bond strength.","authors":"Fikri Öcal, Ayşe Karabaş, Buse Çebi Gül","doi":"10.1016/j.dental.2026.03.160","DOIUrl":"https://doi.org/10.1016/j.dental.2026.03.160","url":null,"abstract":"<p><strong>Objective: </strong>The aim of this study was to compare the rheological parameters, hybrid layer thicknesses, inorganic filler contents determined by thermogravimetric analysis (TGA), and elemental compositions obtained by energy-dispersive X-ray spectroscopy (EDX) of five different universal adhesives (G-Premio Bond [GPB], Clearfil Universal Bond [CUB], Prime Bond Universal [PBU], OptiBond Universal [OBU], and Gluma Bond Universal [GBU]) and to evaluate the relationship of these parameters with microtensile bond strength.</p><p><strong>Materials and methods: </strong>Universal adhesives were applied to dentin specimens obtained from human permanent teeth. Rheological properties were measured with an oscillatory rheometer (0.3 mm gap, 2 Hz, 23 °C) in terms of viscosity, storage modulus, and loss modulus. Adhesive layer thicknesses were measured under a scanning electron microscope at × 1000 magnification, inorganic filler ratios were determined by TGA (30-600 °C), and elemental compositions were assessed by EDX. In addition, microtensile bond strength tests were performed, and the obtained values were compared with rheological, morphological, and chemical parameters.</p><p><strong>Results: </strong>Rheological analysis revealed that CUB exhibited the highest complex viscosity and modulus values, while PBU showed the lowest (p < 0.05). CUB produced the thickest adhesive, whereas PBU had the thinnest. TGA results indicated that OBU had the highest inorganic filler content, and PBU the lowest. Mechanical testing showed that OBU achieved the highest bond strength, while PBU demonstrated the lowest (p < 0.05). Despite showing no significant elemental differences in EDX analysis, GBU, together with GPB, presented the second-highest bond strength.</p><p><strong>Clinical significance: </strong>Microstructural features, compositional characteristics, and rheology-based properties of universal adhesives are important factors influencing both bond strength and adhesive layer formation, and evaluating these parameters together may contribute to more predictable clinical outcomes.</p>","PeriodicalId":298,"journal":{"name":"Dental Materials","volume":" ","pages":""},"PeriodicalIF":6.3,"publicationDate":"2026-03-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147493262","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Biocompatibility of silver and hydroxyapatite antimicrobial nanocoatings on titanium alloy dental implants with human gingival fibroblasts. 银和羟基磷灰石抗菌纳米涂层在人牙龈成纤维细胞钛合金种植体上的生物相容性。

IF 6.3 1区医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE

Dental Materials

Pub Date : 2026-03-20 DOI: 10.1016/j.dental.2026.03.003

S Morgan, R D Handy, V M Salih, R N Salaie, C J Tredwin, A Besinis

Objectives: Peri-implantitis compromises soft and hard tissues around dental implants, often leading to implant failure. Antibacterial nanocoatings offer a promising infection control strategy, but maintaining biocompatibility is essential. This study investigated, through a range of assays and analytical techniques, the biocompatibility of antimicrobial silver and hydroxyapatite (HA) nanocoatings applied to titanium implants with human gingival fibroblasts (HGFs).

Methods: Silver and hydroxyapatite nanocoatings were applied to the surface of titanium alloy specimens using electroplating, deposition and sintering techniques. The biocompatibility of the nanocoatings with HGFs was assessed by measuring cell metabolic activity (alamarBlue), lactate dehydrogenase (LDH) release, collagen production (Sircol assay), and cell morphology (scanning electron microscopy). Nanocoating stability was tested in ultrapure water, Modified Krebs and artificial saliva.

Results: Elevated total Ag⁺ concentrations were measured in the media released from the silver and HA nanocoatings (1.78 mg/l on day 4 and 1 mg/l by day 7). Electrolytes remained within physiological ranges. The HGFs cultured on the nanocoatings showed normal morphology, intact membranes (LDH < 60 nmol/min/ml), healthy collagen secretion (27.18 - 31.11 µg/ml), and aerobic metabolism at 80% of controls, consistent with biocompatibility.

Significance: The silver and HA nanocoatings confirmed a sustained Ag⁺ release, necessary for a strong antimicrobial activity, while maintaining HGFs health and cell functionality. Our previous work has confirmed the strong antimicrobial activity of these nanocoatings when applied to dental implants, and the findings of this study have demonstrated that the implant biocompatibility is not compromised. This suggests that these silver and HA nanocoatings can be safely used to minimise peri-implantitis and prevent implant failure.

目的：种植体周围炎损害种植体周围的软硬组织，经常导致种植体失败。抗菌纳米涂层提供了一种很有前途的感染控制策略，但保持生物相容性是必不可少的。本研究通过一系列的实验和分析技术，研究了抗菌银和羟基磷灰石（HA）纳米涂层应用于人牙龈成纤维细胞（HGFs）钛种植体的生物相容性。方法：采用电镀、沉积和烧结技术在钛合金试样表面制备银纳米涂层和羟基磷灰石纳米涂层。通过测量细胞代谢活性（alamarBlue）、乳酸脱氢酶（LDH）释放、胶原生成（Sircol测定）和细胞形态（扫描电镜）来评估纳米涂层与HGFs的生物相容性。在超纯水、改性Krebs和人工唾液中测试了纳米涂层的稳定性。结果：银和透明质酸纳米涂层释放的介质中总Ag+浓度升高（第4天为1.78 mg/l，第7天为1 mg/l）。电解质保持在生理范围内。在纳米涂层上培养的hgf形态正常，膜完整（LDH < 60 nmol/min/ml），胶原分泌正常（27.18 ~ 31.11 µg/ml），有氧代谢达到对照组的80%，与生物相容性一致。意义：银和透明质酸纳米涂层证实了Ag+的持续释放，这是维持hgf健康和细胞功能的必要条件。我们之前的工作已经证实了这些纳米涂层在应用于牙种植体时具有很强的抗菌活性，而本研究的发现也证明了种植体的生物相容性没有受到损害。这表明这些银和透明质酸纳米涂层可以安全地用于减少种植体周围炎和防止种植体失败。

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引用次数: 0

Functionalized blended 3D-printed artificial bone with adjustable homeostasis for osteoporotic alveolar defect repair. 可调节动态平衡的功能化混合3d打印人工骨用于骨质疏松性牙槽缺损修复。

IF 6.3 1区医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE

Dental Materials

Pub Date : 2026-03-19 DOI: 10.1016/j.dental.2026.03.158

Weimin Zhang, Jiaxin Zhang, Zexin Di, Yang Liu, Xueyu Zhang, Tiansen Pei, Zhaoli Li, Yunlong Huo, Yuxi Jia, Chen Li, He Liu

Repair of osteoporotic alveolar bone defect remains challenging owing to a local microenvironment characterized by impaired osteogenesis and heightened osteoclast activity, which constrains new bone formation. Conventional bone repair materials are ill-equipped to specifically target and modulate this complex milieu, highlighting the urgent need for biomaterials that integrate structural support with microenvironment-responsive, dual regulation of bone remodeling. Here, leveraging the putative coordination interaction between nano-hydroxyapatite (Ca²⁺ sites) and zoledronic acid (ZOL) (phosphonate groups), we endowed a 3D-printed poly(lactic-co-glycolic acid) artificial bone with high drug-loading capacity and sustained, localized delivery-associated with matrix biodegradation and gradual desorption/dissociation of putatively bound ZOL and thereby enhance regeneration of osteoporotic defects. Our results demonstrate that an appropriately dosed ZOL-co-blended printed artificial bone significantly suppresses osteoclast activation-related bone metabolic indices while concomitantly promoting the expression of osteogenic differentiation markers, indicative of bidirectional regulation of bone homeostasis. In an osteoporotic rat distal femoral condyle defect model, the ZOL-blended scaffold markedly improved the volume and quality of newly formed bone under pathological conditions, recalibrated peri-implant bone metabolism, and strengthened implant interfacial bone regeneration. This integrative strategy-uniting 3D-printed architecture, mineral-mimetic chemistry, and localized antiresorptive therapy-offers a clinically promising and potentially translatable solution for the regenerative treatment of osteoporotic alveolar bone defect.

骨质疏松性牙槽骨缺损的修复仍然具有挑战性，因为局部微环境以成骨功能受损和破骨细胞活性升高为特征，这限制了新骨的形成。传统的骨修复材料无法专门针对和调节这种复杂的环境，因此迫切需要将结构支持与微环境响应性骨重塑的双重调节结合起来的生物材料。在这里，利用纳米羟基磷灰石（Ca 2 +位点）和唑来膦酸（ZOL）（膦酸基团）之间假定的配位相互作用，我们赋予了一种3d打印的聚乳酸-羟基乙酸)人工骨，该人工骨具有高载药能力和持续的局部递送——与基质生物降解和假定结合的ZOL的逐渐解吸附/解离相关，从而增强了骨质疏松缺陷的再生。我们的研究结果表明，适当剂量的zol共混打印人工骨显著抑制破骨细胞激活相关的骨代谢指标，同时促进成骨分化标志物的表达，表明骨稳态的双向调节。在骨质疏松大鼠股骨远端髁缺损模型中，zol -混合支架在病理条件下明显改善了新生骨的体积和质量，重新校准了种植体周围骨代谢，增强了种植体界面骨再生。这种结合3d打印结构、模拟矿物化学和局部抗吸收治疗的综合策略，为骨质疏松性牙槽骨缺损的再生治疗提供了一种具有临床前景和潜在可转化性的解决方案。

{"title":"Functionalized blended 3D-printed artificial bone with adjustable homeostasis for osteoporotic alveolar defect repair.","authors":"Weimin Zhang, Jiaxin Zhang, Zexin Di, Yang Liu, Xueyu Zhang, Tiansen Pei, Zhaoli Li, Yunlong Huo, Yuxi Jia, Chen Li, He Liu","doi":"10.1016/j.dental.2026.03.158","DOIUrl":"https://doi.org/10.1016/j.dental.2026.03.158","url":null,"abstract":"<p><p>Repair of osteoporotic alveolar bone defect remains challenging owing to a local microenvironment characterized by impaired osteogenesis and heightened osteoclast activity, which constrains new bone formation. Conventional bone repair materials are ill-equipped to specifically target and modulate this complex milieu, highlighting the urgent need for biomaterials that integrate structural support with microenvironment-responsive, dual regulation of bone remodeling. Here, leveraging the putative coordination interaction between nano-hydroxyapatite (Ca²⁺ sites) and zoledronic acid (ZOL) (phosphonate groups), we endowed a 3D-printed poly(lactic-co-glycolic acid) artificial bone with high drug-loading capacity and sustained, localized delivery-associated with matrix biodegradation and gradual desorption/dissociation of putatively bound ZOL and thereby enhance regeneration of osteoporotic defects. Our results demonstrate that an appropriately dosed ZOL-co-blended printed artificial bone significantly suppresses osteoclast activation-related bone metabolic indices while concomitantly promoting the expression of osteogenic differentiation markers, indicative of bidirectional regulation of bone homeostasis. In an osteoporotic rat distal femoral condyle defect model, the ZOL-blended scaffold markedly improved the volume and quality of newly formed bone under pathological conditions, recalibrated peri-implant bone metabolism, and strengthened implant interfacial bone regeneration. This integrative strategy-uniting 3D-printed architecture, mineral-mimetic chemistry, and localized antiresorptive therapy-offers a clinically promising and potentially translatable solution for the regenerative treatment of osteoporotic alveolar bone defect.</p>","PeriodicalId":298,"journal":{"name":"Dental Materials","volume":" ","pages":""},"PeriodicalIF":6.3,"publicationDate":"2026-03-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147490319","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Reproducibility of accelerated fatigue test of dentin-composite discs under cyclic diametral compression. 牙本质复合材料圆盘在循环直径压缩下加速疲劳试验的再现性。

IF 6.3 1区医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE

Dental Materials

Pub Date : 2026-03-19 DOI: 10.1016/j.dental.2026.03.157

Daniel Larrañaga-Ordaz, Ruoqiong Chen, Bonita VanHeel, Lin Zhang, Bruno P Lima, Hooi Pin Chew, Alex Fok

Objectives: This study considers the reproducibility of a newly proposed Medical Device Development Tool (MDDT) for testing the durability of the tooth-restoration interface in dental resin-composite restorations.

Methods: The tool is in the form of an accelerated fatigue test using dentin-composite discs subjected to cyclic diametral compression with a linearly increasing load amplitude. Three operators performed the test separately, with each using 30 specimens.

Results: The 3 runs produced very similar mean numbers of cycles to failure as well as survival probability plots, demonstrating the test's reproducibility. Geometric analyses did not show any strong association between dimensional variations and the number of cycles to failure. Fatigue parameters derived from the test results also agreed with some of those reported in the literature based on beams in 4-point bending.

Significance: The proposed MDDT is a reproducible and reliable durability test for resin-composite systems.

目的：本研究考虑了一种新提出的医疗器械开发工具（MDDT）的可重复性，用于测试牙科树脂复合修复体中牙齿-修复体界面的耐久性。方法：该工具采用加速疲劳试验的形式，使用牙本质复合材料盘进行循环直径压缩，加载幅度线性增加。三名操作员分别进行测试，每人使用30个标本。结果：3次运行产生了非常相似的平均失败周期数以及生存概率图，证明了测试的可重复性。几何分析没有显示出尺寸变化和失效循环次数之间有任何强烈的联系。根据试验结果得出的疲劳参数也与文献中基于4点弯曲的梁的一些报告一致。意义：所提出的MDDT是一种可重复的、可靠的树脂复合材料耐久性试验。

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引用次数: 0