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Objectives: The objectives of this study were to: (1) develop a multifunctional adhesive via dimethylaminohexadecyl methacrylate (DMAHDM) and nanoparticles of amorphous calcium phosphate (NACP); and (2) investigate its ability to provide metalloproteinases (MMPs) deactivation and remineralization for long-term dentin bonding durability., Methods: DMAHDM and NACP were incorporated into Adper™ Single Bond 2 Adhesive (SB2) at mass fractions of 5% and 20%, respectively. Degree of conversion and contact angle were measured. Endogenous MMP activity of the demineralized dentin beams, Masson's trichrome staining, nano-indentation, microtensile bond strength and interfacial nanoleakage analyses were investigated after 24 h and 3 months of storage aging in artificial saliva., Results: Adding DMAHDM and NACP did not compromise the degree of conversion and contact angle of SB2 (p > 0.05). DMAHDM and NACP incorporation reduced the endogenous MMP activity by 53 %, facilitated remineralization, and increased the Young's modulus of hybrid layer by 49 % after 3 months of aging in artificial saliva, compared to control. For SB2 Control, the dentin bond strength decreased by 38 %, with greater nanoleakage expression, after 3 months of aging (p < 0.05). However, DMAHDM+NACP group showed no loss in bond strength, with much less nanoleakage, after 3 months of aging (p > 0.05)., Significance: DMAHDM+NACP adhesive greatly reduced MMP-degradation activity in demineralized dentin, induced remineralization at adhesive-dentin interface, and maintained the dentin bond strength after aging, without adversely affecting polymerization and dentin wettability. This new adhesive has great potential to help eliminate secondary caries, prevent hybrid layer degradation, and increase the resin-dentin bond longevity., (Copyright © 2022 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.)

Objectives: This study aimed to develop an antibacterial and calcium (Ca) and phosphate (P) rechargeable adhesive and investigate the effects of dimethylaminododecyl methacrylate (DMAHDM) and nanoparticles of amorphous calcium phosphate (NACP) on dentin bonding, biofilm response, and repeated Ca and P ion recharge and re-release capability for the first time., Materials and Methods: Pyromellitic glycerol dimethacrylate (PMGDM), ethoxylated bisphenol A dimethacrylate (EBPADMA), 2-hydroxyethyl methacrylate (HEMA), and bisphenol A glycidyl dimethacrylate (BisGMA) formed the adhesive (PEHB). Three groups were tested: (1) Scotchbond (SBMP, 3 M) control, (2) PEHB + 30% NACP, and (3) PEHB + 30% NACP + 5% DMAHDM. Specimens were tested for dentin shear bond strength, and Ca and P ion release, recharge, and re-release. Biofilm lactic acid production and colony-forming units (CFU) on resins were analyzed., Results: The four groups had similar dentin shear bond strengths (p > 0.1). Adhesive with DMAHDM showed significant decrease in metabolic activity, lactic acid production, and biofilm CFU (p < 0.05). The adhesives containing NACP released high levels of Ca and P ions initially and after being recharged., Conclusion: This study developed the first Ca and P ion-rechargeable and antibacterial adhesive, achieving strong antibacterial activity and Ca and P ion recharge and re-release for long-term remineralization., Clinical Relevance: Considering the restoration-tooth bonded interface being the weak link and recurrent caries at the margins being the primary reason for restoration failures, this novel calcium phosphate-rechargeable and antibacterial adhesive is promising for a wide range of tooth-restoration applications to inhibit caries., (© 2021. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)

Objective: Dentin remineralization at the bonded interface would protect it from external risk factors, therefore, would enhance the longevity of restoration and combat secondary caries. Dental biofilm, as one of the critical biological factors in caries formation, should not be neglected in the assessment of caries preventive agents. In this work, the remineralization effectiveness of demineralized human dentin in a multi-species dental biofilm environment via an adhesive containing nanoparticles of amorphous calcium phosphate (NACP) and dimethylaminohexadecyl methacrylate (DMAHDM) was investigated., Methods: Dentin demineralization was promoted by subjecting samples to a three-species acidic biofilm containing Streptococcus mutans, Streptococcus sanguinis, Streptococcus gordonii for 24h. Samples were divided into a control group, a DMAHDM adhesive group, an NACP group, and an NACP+DMAHDM adhesive group. A bonded model containing a control-bonded group, a DMAHDM-bonded group, an NACP-bonded group, and an NACP+DMAHDM-bonded group was also included in this study. All samples were subjected to a remineralization protocol consisting of 4-h exposure per 24-h period in brain heart infusion broth plus 1% sucrose (BHIS) followed by immersion in artificial saliva for the remaining period. The pH of BHIS after 4-h immersion was measured every other day. After 14 days, the biofilm was assessed for colony-forming unit (CFU) count, lactic acid production, live/dead staining, and calcium and phosphate content. The mineral changes in the demineralized dentin samples were analyzed by transverse microradiography., Results: The in vitro experiment results showed that the NACP+DMAHDM adhesive effectively achieved acid neutralization, decreased biofilm colony-forming unit (CFU) count, decreased biofilm lactic acid production, and increased biofilm calcium and phosphate content. The NACP+DMAHDM adhesive group had higher remineralization value than the NACP or DMAHDM alone adhesive group., Significance: The NACP+DMAHDM adhesive was effective in remineralizing dentin lesion in a biofilm model. It is promising to use NACP+DMAHDM adhesive to protect bonded interface, inhibit secondary caries, and prolong the longevity of restoration., (Copyright © 2020 The Academy of Dental Materials. All rights reserved.)

Objectives: Fluoride-containing orthodontic cements are used to combat white spot lesions (WSLs) in enamel. However, the fluoride (F) ion releases from these cements are relatively low and short-term. The objectives of this study were to develop a novel rechargeable orthodontic cement with nanoparticles of calcium fluoride (nCaF 2 ) to provide long-term and high levels of F release, and to investigate F recharge and physical and cytotoxic properties., Methods: The nCaF 2 with a mean particle size of 58 nm were synthesized using a spray-drying method. Pyromellitic glycerol dimethacrylate (PMGDM), ethoxylated bisphenol A dimethacrylate (EBPADMA), 2-hydroxyethyl methacrylate (HEMA) and bisphenol A glycidyl dimethacrylate (BisGMA) were used to prepare the cements (denoted PE and PEHB resins). A resin-modified glass ionomer (RMGI) served as control. Enamel shear bond strength (SBS), cytotoxicity, and F ion recharge and re-release were evaluated., Results: nCaF 2 cements had good SBS and excellent biocompatibility that were comparable to RMGI (p > 0.1). After a recharge for 1 min, the F re-release from PEHB + 30%nCaF 2 cement was 80% higher than RMGI (p < 0.05). Increasing nCaF 2 content from 20% to 30% greatly increased the F ion re-release (p < 0.05). The F ion re-release of nCaF 2 cements did not decrease with increasing the number of recharge and re-release cycles (p > 0.1)., Conclusions: A novel F ion-rechargeable orthodontic cement containing nCaF 2 was developed with clinically acceptable enamel SBS, good biocompatibility, and sustained F ion recharge and re-release that were 1.8 folds that of a commercial RMGI., Clinical Significance: Novel rechargeable nCaF 2 orthodontic cement is promising to provide the needed long-term and high levels of F ion releases to inhibit WSLs in orthodontics., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Objectives: The remineralization of dentin at a bonded interface would help to strengthen the bonded interface and inhibit secondary caries, and would prolong the longevity of restoration. The aim of this study was to investigate the remineralization of demineralized human dentin in a dental biofilm environment via an adhesive containing nanoparticles of amorphous calcium phosphate (NACP)., Methods: Dentin demineralization was promoted by subjecting samples to a Streptococcus mutans acidic biofilm for 24 h. Samples were divided into a control group, a commercial fluoride-releasing adhesive group, and an NACP adhesive group. All samples were subjected to a remineralization protocol consisting of 4-h exposure per 24-h period in brain heart infusion broth plus 1% sucrose (BHIS) followed by immersion in artificial saliva for the remaining period. The pH of BHIS after 4-h immersion was measured every other day. After 10 days, the biofilm was assessed for colony-forming unit (CFU) count, lactic acid production, live/dead staining, and calcium and phosphate content. The mineral changes in the demineralized dentin samples were analyzed by transverse microradiography, hardness measurement, X-ray diffraction characterization, and scanning electron microscopy., Results: The NACP adhesive achieved acid neutralization, decreased biofilm CFU count, decreased biofilm lactic acid production, and increased biofilm calcium and phosphate content (P < 0.05). The NACP adhesive group had higher remineralization value than the commercial fluoride-releasing adhesive group (P < 0.05)., Conclusions: The NACP adhesive was effective in remineralizing dentin lesions in a biofilm model. Its ability to protect bond interface, inhibit secondary caries, and prolong the longevity of restoration is promising., Clinical Significance: Using NACP-containing adhesives could be recommended because of the protective ability of its hybrid layer even under a biofilm-challenged environment., (Copyright © 2019. Published by Elsevier Ltd.)

Objectives: The objectives of this study were to develop a resin-modified glass ionomer containing nanoparticles of calcium fluoride (nCaF 2 ) and dimethylaminohexadecyl methacrylate (DMAHDM) for the first time and investigate the antibacterial and remineralization properties., Methods: nCaF 2 was synthesized using a spray-drying method and characterized using a transmission electron microscope. Twenty weight percentage (wt%) nCaF 2 and 3 wt% DMAHDM were incorporated into a RMGI (GC Ortho LC). Enamel shear bond strength (SBS) and cytotoxicity were determined. Fluoride (F) and calcium (Ca) ion releases were assessed. Biofilm live/dead staining, metabolic activity, polysaccharide and lactic production, and colony-forming units (CFU) were evaluated. The remineralization ability was determined by measuring the effects of cements on enamel surface hardness and lesion depth., Results: Incorporating 20 wt% nCaF 2 and 3 wt% DMAHDM did not compromise the SBS (p > 0.1). The decrease of pH from 7.0 to 4.0 significantly increased the F and Ca ion releases. The new cement greatly reduced the metabolic activity, polysaccharide and lactic acid productions, and lowered the biofilm CFU by 3 log, compared to commercial control (p < 0.05). The new cement increased the enamel hardness by 56% and decreased the lesion depth by 43%, compared to control (p < 0.05). The cell viability at 7 days against the new cement extracts was 82.2% of that of the negative control in culture medium without any extracts., Conclusions: The novel orthodontic cement containing nCaF 2 and DMAHDM achieved much stronger antibacterial and remineralization capabilities and greater enamel hardness than the commercial control did, without compromising the orthodontic bracket-enamel SBS and biocompatibility., Clinical Significance: The novel bioactive and nanostructured orthodontic cement is promising to inhibit enamel demineralization, white spot lesions and caries in orthodontic treatments., (Published by Elsevier Ltd.)

Objective: Secondary caries and micro-cracks are the main limiting factors for dentin bond durability. The objectives of this study were to develop a self-healing adhesive containing dimethylaminohexadecyl methacrylate (DMAHDM) and nanoparticles of amorphous calcium phosphate (NACP), and investigate the effects of water-aging for 12 months on self-healing, dentin bonding, and antibacterial properties for the first time., Methods: Microcapsules were synthesized with poly (urea-formaldehyde) (PUF) shells containing triethylene glycol dimethacrylate (TEGDMA) and N,N-dihydroxyethyl-p-toluidine (DHEPT). The adhesive contained 7.5% microcapsules, 10% DMAHDM, and 20% NACP (all mass). Specimens were water-aged at 37 °C for 1 day to 12 months. Dentin bond strength was measured using extracted human teeth. A single-edge-V-notched-beam (SEVNB) method was used to measure fracture toughness K IC and self-healing efficiency. A dental plaque microcosm biofilm model was used with human saliva as inoculum., Results: The microcapsules + DMAHDM + NACP group showed no decline in dentin bond strength after water-aging for 12 months, which was significantly higher than that of other groups without DMAHDM (p < 0.05). A self-healing efficiency of 67% recovery in K IC was obtained even after 12 months of water immersion, indicating that the self-healing ability was not lost in water-aging (p > 0.1). The bacteria-killing ability of this adhesive did not decline from 1 day to 12 months (p > 0.1), with biofilm CFU reduction by 3-4 orders of magnitude after the resin was water-aged for 12 months, compared to control resin., Significance: This novel adhesive with triple merits of self-healing, antibacterial and remineralization functions showed an excellent long-term durability in water-aging for 12 months. This multifunctional adhesive has the potential for dental applications to heal cracks, inhibit bacteria, provide ions for remineralization, and increase the restoration longevity., (Copyright © 2019 The Academy of Dental Materials. All rights reserved.)

Cariogenic oral biofilms are strongly linked to dental caries around dental sealants. Quaternary ammonium monomers copolymerized with dental resin systems have been increasingly explored for modulation of biofilm growth. Here, we investigated the effect of dimethylaminohexadecyl methacrylate (DMAHDM) on the cariogenic pathogenicity of Streptococcus mutans ( S. mutans ) biofilms. DMAHDM at 5 mass% was incorporated into a parental formulation containing 20 mass% nanoparticles of amorphous calcium phosphate (NACP). S. mutans biofilms were grown on the formulations, and biofilm inhibition and virulence properties were assessed. The tolerances to acid stress and hydrogen peroxide stress were also evaluated. Our findings suggest that incorporating 5% DMAHDM into 20% NACP-containing sealants (1) imparts a detrimental biological effect on S. mutans by reducing colony-forming unit counts, metabolic activity and exopolysaccharide synthesis; and (2) reduces overall acid production and tolerance to oxygen stress, two major virulence factors of this microorganism. These results provide a perspective on the value of integrating bioactive restorative materials with traditional caries management approaches in clinical practice. Contact-killing strategies via dental materials aiming to prevent or at least reduce high numbers of cariogenic bacteria may be a promising approach to decrease caries in patients at high risk.

Objectives: The objective of the present study was to investigate long-term dentin remineralization via the combination of poly(amido amine) (PAMAM) with a novel rechargeable adhesive containing nanoparticles of amorphous calcium phosphate (NACP)., Methods: The NACP adhesive was immersed in lactic acid at pH 4 to exhaust its calcium (Ca) and phosphate (P) ion release, and then recharged with Ca and P ions. Dentin samples were pre-demineralized with 37% phosphoric acid, and then divided into four groups: (1) dentin control, (2) dentin treated with PAMAM, (3) dentin with recharged NACP adhesive, (4) dentin with PAMAM + recharged NACP adhesive. In group (2) and (4), the PAMAM-coated dentin was immersed in phosphate-buffered saline with vigorous shaking for 77 days to accelerate any detachment of the PAMAM macromolecules from the demineralized dentin. Samples were treated with a cyclic remineralization/demineralization regimen for 21 days., Results: After 77 days of fluid flow challenge, the immersed PAMAM still retained its nucleation template function. The recharged NACP adhesive possessed sustained ion re-release and acid-neutralization capability, both of which did not decrease with repeated recharge and re-release cycles. The immersed PAMAM with the recharged NACP adhesive achieved long-term dentin remineralization, and restored dentin hardness to that of healthy dentin., Conclusions: The PAMAM + NACP adhesive completely remineralizes pre-demineralized dentin even after long-term fluid challenges and provides long-term remineralization to protect tooth structures., Clinical Significance: The novel PAMAM + NACP adhesive provides long-term bond protection and caries inhibition to increase the longevity of resin-based restorations., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

The objectives were to develop a novel rechargeable cement containing amorphous calcium-phosphate nanoparticles (nanoACP) to suppress tooth decay. Five cements were made with: (1) 60% glass particles (experimental control); (2) 40% glass+20% nanoACP; (3) 30% glass+30% nanoACP; (4) 20% glass+40% nanoACP; (5) 10% glass+50% nanoACP. Groups 1-4 had enamel bond strengths similar to Transbond XT (3M) and Vitremer (3M) (p>0.1). The nanoACP cement had calcium and phosphate ion release which increased with increasing nanoACP fillers. The recharged cement had substantial ion re-release continuously for 14 days after a single recharge. Ion re-release did not decrease with increasing recharge/re-release cycles. Groups 3-5 maintained a safe pH of medium (>5.5); however, control cements had cariogenic pH of medium (<4.5) due to biofilm acid. Therefore, nanoACP cement (1) had good bond strength to enamel, (2) possessed calcium and phosphate ion recharge/re-release capability, and (3) raised biofilm pH to a safe level to inhibit caries.

Objectives: The dentin bonding often fails over time, leading to secondary caries and restoration failure. The objectives of this study were to develop an adhesive with dimethylaminohexadecyl methacrylate (DMAHDM) and nanoparticles of amorphous calcium phosphate (NACP), and investigate the effects of storage in artificial saliva for six months on the bonding durability, antibacterial activity, ion release and biofilm pH properties for the first time., Methods: DMAHDM was added at 5% (by mass) to Scotchbond Primer and Adhesive (SBMP). NACP was added at 10%, 20%, and 30% to SBMP adhesive. Dentin bonding durability, antibacterial activity against Streptococcus mutans biofilms, and calcium (Ca) and phosphate (P) ion liberation properties were investigated after 1 day and 6months of storage in artificial saliva., Results: Dentin bond strength (n = 50) had 25% loss after 6 months of aging for SBMP control. However, SBMP + DMAHDM+10NACP and SBMP + DMAHDM+20NACP showed no loss in bond strength after storage in artificial saliva for 6 months. The DMAHDM + NACP incorporation method dramatically reduced the biofilm metabolic activity and acid production, and decreased the biofilm CFU by four orders of magnitude, compared to SBMP control, even after 6 months of aging (p < 0.05). DMAHDM + NACP had long-lasting Ca and P ion releases, and raised the biofilm pH to 6.8, while the control group had a cariogenic biofilm pH of 4.5., Conclusions: Incorporating DMAHDM + NACP in bonding agent yielded potent and long-lasting antibacterial activity and ions liberation ability, and much higher long-term dentin bond strength after 6-month of aging. The new bonding agent is promising to inhibit caries at the restoration margins and increase the resin-dentin bonding longevity., Clinical Significance: The novel bioactive adhesive is promising to protect tooth structures from biofilm acids and secondary caries. NACP and DMAHDM have great potential for applications to a wide range of dental materials to reduce plaque and achieve therapeutic effects., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Enamel demineralization is the most undesired side-effect of fixed orthodontic treatments. This study were to develop a novel adhesive that is self-etching instead of using the traditional etching method, and to form a sealant on the enamel to prevent demineralization. 2-methacryloyloxyethyl phosphorylcholine (MPC) and quaternary ammonium dimethylaminohexadecyl methacrylate (DMAHDM) were mixed into a self-etch adhesive (Adper Easy One, 3M, St. Paul, MN, USA; referred to as AEO). Enamel shear bond strength (SBS) was measured. Protein adsorption onto the resins was measured. An oral microcosm biofilm model with saliva was tested. Incorporation of 7.5% MPC and 5% DMAHDM into AEO did not reduce the SBS (p>0.1). AEO with 7.5% MPC+5% DMAHDM had protein adsorption that was only 1/18 that of AEO control. AEO with 7.5% MPC+5% DAMHDM had much stronger antibacterial properties (p<0.05). In conclusion, the new self-etch adhesive with MPC and DAMHDM greatly reduced protein adsorption and inhibited biofilm viability.

Objectives: The objectives were to develop a calcium (Ca) and phosphate (P) ion-rechargeable and protein-repellent adhesive containing nanoparticles of amorphous calcium phosphate (NACP) and 2-methacryloyloxyethyl phosphorylcholine (MPC), and investigate the MPC effects on ion recharge and re-releases for the first time., Methods: Pyromellitic glycerol dimethacrylate and ethoxylated bisphenol-A dimethacrylate were used to fabricate adhesive PEHB. Six adhesives were tested: (1) Scotchbond (SBMP); (2) PEHB, (3) PEHB + 20%NACP; (4) PEHB + 30%NACP; (5) PEHB + 20%NACP+3%MPC; (6) PEHB + 30%NACP+3%MPC. Dentin shear bond strength, Ca/P ion release, recharge and re-release, and protein adsorption were measured. A microcosm biofilm model was tested for lactic-acid production and colony-forming units (CFU)., Results: Adding NACP + MPC did not negatively affect dentin bond strength (p > 0.1). With increasing the number of recharge/re-release cycles, the Ca/P ion re-release reached similarly higher levels (p > 0.1), indicating long-term remineralization capability. One recharge enabled the adhesives to have continued re-releases for 21 days. Incorporation of 3% MPC yielded 10-fold decrease in protein adsorption, and 1-2 log decrease in biofilm CFU., Conclusions: The new rechargeable adhesive with MPC + 30%NACP greatly reduced protein adsorption, biofilm growth and lactic acid. Incorporation of MPC did not compromise the excellent Ca/P ion release, rechargeability, and dentin bond strength., Clinical Significance: Novel bioactive adhesive containing MPC + NACP is promising to repel proteins and bacteria, and inhibit secondary caries at the restoration margins. The method of NACP + MPC to combine CaP-recharge and protein-repellency is applicable to the development of a new generation of materials including composites and cements to suppress oral biofilms and plaque formation and protect tooth structures., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Introduction: The purpose of this study was to investigate the physical and antibacterial properties of a resin sealer mixed with a quaternary ammonium compound, dimethylaminododecyl methacrylate (DMAHDM) and nanosilver (NAg)., Methods: A pilot study was completed to determine the highest concentrations of DMAHDM and NAg that did not significantly alter the physical properties (setting time, flow, solubility, and dimensional change) of AH Plus (Dentsply Sirona, York, PA) when added to the sealer. These concentrations were selected to create a modified resin sealer (mAH Plus). A modified direct contact test evaluated antibacterial properties of AH Plus, DMAHDM + AH Plus, NAg + AH Plus, and mAH Plus at days 1, 7, and 14 against Enterococcus faecalis., Results: Concentrations of 2.5% DMAHDM and 0.15% NAg were added to AH Plus. The flow of mAH Plus was significantly decreased but still within American National Standards Institute/American Dental Association specifications. There were no significant differences in setting time, solubility, or dimensional change. On day 1, 0.15% NAg + AH Plus, 2.5% DMAHDM + AH Plus, and mAH Plus were significantly more effective against E. faecalis compared with AH Plus (P < .05). On days 7 through 14, 2.5% DMAHDM + AH Plus and mAH Plus continued to be significantly more antibacterial than AH Plus (P < .05)., Conclusions: The addition of 0.15% NAg and 2.5% DMAHDM did not adversely affect the physical properties of AH Plus, and mAH Plus was significantly more antibacterial against E. faecalis., (Copyright © 2018 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.)

Patients with dry mouth often have an acidic oral environment lacking saliva to provide calcium (Ca) and phosphate (P) ions. There has been no report on tooth remineralization in acidic pH4 and CaP ion-lacking solutions. The objective of this study was to develop a novel method of combining poly(amido amine) (PAMAM) with adhesive containing nanoparticles of amorphous calcium phosphate (NACP) for dentin remineralization in pH4 and CaP-lacking solution for the first time. Demineralized dentin was tested in four groups: (1) dentin control, (2) dentin with PAMAM, (3) dentin with NACP adhesive, (4) dentin with PAMAM + NACP adhesive. Dentin samples were examined by scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS) and hardness testing. Increasing the NACP filler level in adhesive from 0 to 40 wt% did not negatively affect the dentin bond strength (p > 0.1). NACP adhesive released CaP ions and neutralized the acid. PAMAM alone failed to achieve dentin remineralization in lactic acid. NACP alone induced slight dentin remineralization in lactic acid (p > 0.1). In contrast, the novel PAMAM + NACP group in the pH4 and CaP-lacking solution completely remineralized the predemineralized dentin, increasing its hardness which approached that of healthy dentin (p > 0.1). In conclusion, dentin remineralization via PAMAM + NACP adhesive in pH4 and CaP-lacking acid was achieved for the first time, when conventional remineralization methods such as PAMAM or NACP did not work. The novel PAMAM + NACP method is promising to increase the longevity of the composite-tooth bond, inhibit caries, remineralize lesions and protect tooth structures, even for patients with dry mouth and an acidic oral environment. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 106B: 2414-2424, 2018., (© 2017 Wiley Periodicals, Inc.)

Objectives: Secondary caries at the tooth-restoration margins is a primary reason for restoration failure. Cracks at the margins lead to leakage which can trap bacteria, producing acids to cause caries. To date, there has been no report on developing an adhesive resin that has self-healing, antibacterial and remineralizing capabilities. The objectives of this study were to: (1) develop the first self-healing adhesive with antimicrobial and remineralizing capabilities, and (2) investigate the effects of incorporating microcapsules, dimethylaminohexadecyl methacrylate (DMAHDM) and nanoparticles of amorphous calcium phosphate (NACP) for the first time., Methods: Self-healing microcapsules were synthesized with poly(urea-formaldehyde) (PUF) shells containing triethylene glycol dimethacrylate (TEGDMA) as the healing liquid. The new adhesive contained 7.5% microcapsules, 10% DMAHDM and 20% NACP. A single edge V-notched beam (SEVNB) method was used to measure the fracture toughness K IC and the autonomous crack-healing efficiency. An oral plaque microcosm biofilm model was tested., Results: The new self-healing, antimicrobial and remineralizing dental adhesive matched the dentin bond strength of a commercial control (p > 0.1). The new adhesive achieved successful crack-healing, with an excellent K IC recovery of 67%. The new adhesive had strong antimicrobial activity, reducing biofilm colony-forming units by four orders of magnitude, and reducing biofilm acid production to 1/100th that of biofilms on the commercial control resin., Conclusions: A self-healing adhesive with antibacterial and remineralizing capabilities was developed for the first time. Excellent dentin bond strength, autonomous crack-healing and K IC recovery, and strong anti-biofilm properties were achieved for the new adhesive resin., Clinical Significance: The novel method of using triple agents (self-healing microcapsules + DMAHDM + NACP) is promising for applications in dental adhesives, cements, sealants and composites to combat the two main challenges: fracture and secondary caries., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Enamel demineralization is one of the most undesired side effects of fixed orthodontic treatment, which will lead to white spot lesions (WSLs) on tooth surfaces. The development of WSLs is due to prolonged accumulation of bacterial plaque and associated acid production. Self-etching adhesives have been used in orthodontic treatments with several advantages over the more traditional acid-etch method. However, current self-etching adhesives in orthodontic treatments have no antibacterial activity. The objectives of this study were to develop a self-etching and antibacterial orthodontic adhesive, and to investigate its enamel bond strength and antibacterial properties. A novel quaternary ammonium monomer dimethylaminohexadecyl methacrylate (DMAHDM) was incorporated into a commercial self-etching adhesive (Adper Easy One, 3M). It showed that the 5% DMAHDM appeared to be optimal in obtaining the strongest antibacterial function without compromising the enamel bond strength both at 15 min and after 30 days of immersion plus thermal cycling.

Objectives: To evaluate the bonding performance, antibacterial activity, and remineralization effect on enamel of the orthodontic adhesive containing MAE-DB and NACP., Methods: Eighty non-carious human premolars were divided into 3 groups: Transbond XT (TB), PEHB + 5% MAE-DB (PD), and PEHB + 40% NACP + 5% MAE-DB (PND). Premolars were bonded with orthodontic brackets, the first subgroup (n = 10) and the second subgroup (n = 10) were subjected to shear bond strength testing after immersed in water for 1 day and in demineralization solution for 28 days respectively and then tested surface roughness, while the third subgroup (n = 6) was used for microhardness evaluation after aged in demineralization solution for 28 days. For each adhesive, fifty disk samples were prepared for antibacterial study. Specimens measuring 12 mm × 2 mm × 2 mm were fabricated for ion release test., Results: Bond strengths were in the order TB = PND > PND = PD for "1-day in water", and in the order TB = PND > PD for "28-days in pH 4 solution". No significant difference in the ARI scores for the three adhesive. Numerous bacteria adhered to TB surface, while PD and PND had minimal bacterial growth and activity. PND showed high levels of Ca and P ions release and enamel hardness. The surface roughness of enamel in PND was much lower than TB and PD and showed no significant difference with the sound, control enamel., Conclusion: PND adhesive with 5% MAE-DB and 40% NACP exhibits antibacterial and remineralizing capabilities, and did not adversely affect bond strength compared to commercial adhesive., Clinical Significance: Novel adhesive containing quaternary ammonium monomer and nano-amorphous calcium phosphate represents a promising candidate in combating enamel white spot lesions and even dental caries., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Objectives: A new quaternary ammonium monomer (QAM), triethylaminododecyl acrylate (TEADDA) was synthesized, in which the position of the functional groups was different from that of dimethylaminododecyl methacrylate (DMADDM). The objectives were to: (1) investigate the effect of the changed position of the functional groups on the mechanical properties, anti-biofilm activity and biocompatibility of adhesive resin, and (2) study the anti-bacterial mechanism of QAM to improve the performance of the adhesive system modified by QAM., Methods: TEADDA and DMADDM were added into adhesives. Microtensile bond strength and surface charge density were measured. Multi-species biofilms were incubated on specimens for 16h, 48h and 72h and analyzed via MTT assay, lactic acid measurement and confocal laser scanning microscopy. The ratio of different species of bacteria was measured by real-time polymerase chain reaction. Cytotoxicity and biocompatibility were analyzed by eluents cytotoxicity test and histological images of H&E staining via an animal study in rats., Results: The mass fraction of TEDDA allowed to be added into adhesive was higher than that of DMADDM. However, even 10% TEADDA did not yield a strong anti-biofilm effect on biofilm growth, lactic acid production and bacteria compositions. TEADDA added into adhesives showed better mechanical properties but weaker anti-bacterial effect. There was no significant difference on cytotoxicity and biocompatibility between DMADDM and TEADDA., Significance: The study could be helpful for the investigation of the anti-caries mechanism of QAMs, the design of new QAMs and the improvement of the anti-caries activity of the modified dental materials., (Copyright © 2017 The Academy of Dental Materials. All rights reserved.)

We investigated the anticaries properties of an adhesive containing dimethylaminododecyl methacrylate (DMADDM) in vivo via a secondary caries animal model. Cavities were prepared in the maxillary first molars of Wistar rats. DMADDM-containing adhesives were applied on one side and commercial adhesives on the opposite side as a control. After a 3-week feeding period to induce secondary caries, the molars were harvested for the evaluation of the secondary caries. Lesion depth (LD) and mineral loss (ML) were measured via a micro-CT method, and a modified Keyes scoring method yielded scores for the caries lesions. Statistical analysis was divided into 2 parts: a correlation analysis between 2 evaluations with one-way ANOVA and a least-significant differences (LSD) test, and an evaluation of anticaries adhesives with a paired samples t test. The results showed that: (1) secondary caries was successfully produced in rats; (2) there was a correlation between the modified Keyes scoring method and micro-CT in the evaluation of the secondary caries; (3) the adhesive containing DMADDM significantly reduced both LD and ML (according to micro-CT), and also lowered the scores (based on the modified Keyes scoring method). This suggests that the novel DMADDM adhesive could perform an anticaries function in vivo via the secondary caries animal model which was also developed and testified in research. Secondary caries is one of the major reasons leading to the failure of caries restoration treatment. As a solution, anticaries adhesives perform well in biofilm inhibition in vitro. However, the lack of secondary caries animal models limits the evaluation of anticaries adhesives in vivo., (© 2017 The Author(s) Published by S. Karger AG, Basel.)

Enamel demineralization is destructive, esthetically compromised, and costly complications for orthodontic patients. Nano-sized amorphous calcium phosphate (NACP) has been explored to address this challenge. The 20% NACP-loaded ortho-cement notably exhibited favorable behavior on reducing demineralization of enamel around brackets in a caries model designed to simulate the carious attack. The 20% NACP-loaded ortho-cement markedly promotes higher calcium and phosphate release at a low pH, and the mineral loss was almost two fold lower and carious lesion depth decreased the by 1/3. This novel approach is promising co-adjuvant route for prevention of dental caries dissemination in millions of patients under orthodontic treatment.

Objectives: Dental luting cements are widely used to bond indirect restorations to teeth. Microcracks often lead to cement failures. The objectives of this study were to develop the first self-healing luting cement, and investigate dentin bond strength, mechanical properties, crack-healing, and self-healing durability in water-aging for 6 months., Methods: Microcapsules of poly(urea-formaldehyde) (PUF) shells with triethylene glycol dimethacrylate (TEGDMA) as healing liquid were synthesized. Cement contained bisphenol A glycidyl dimethacrylate, TEGDMA, 4-methacryloyloxyethyl trimellitic and glass fillers. Microcapsules were added at 0%, 2.5%, 5%, 7.5%, 8.5%, 9.5% and 10%. Dentin shear bond strength was measured using extracted human teeth. Flexural strength and elastic modulus were measured. Single edge V-notched beams were used to measure fracture toughness (K IC ) and self-healing. Specimens were water-aged at 37°C for 6 months and then tested for self-healing durability., Results: Adding 7.5% microcapsules into cement achieved effective self-healing, without adverse effects on dentin bond strength and virgin mechanical properties (p>0.1). Excellent self-healing of 68%-77% recovery was obtained. Six months of water-aging did not decrease the self-healing efficiency, compared to 1 d (p>0.1), indicating that the self-healing property did not degrade in water-aging., Conclusions: A self-healing dental luting cement was developed for the first time. It contained fine microcapsules and exhibited an excellent self-healing efficiency, even after being immersed in water for 6 months., Clinical Significance: The self-healing cement is promising for cementing crowns and bridges and other adhesive cement applications, to heal cracks and increase restoration longevity., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

Orthodontic treatments increase the incidence of white spot lesions. The objectives of this study were to develop an antibacterial orthodontic cement to inhibit demineralization, and to evaluate its enamel shear bond strength and anti-biofilm properties. Novel antibacterial monomer dimethylaminohexadecyl methacrylate (DMAHDM) was synthesized and incorporated into Transbond XT at 0, 1.5 and 3% by mass. Anti-biofilm activity was assessed using a human dental plaque microcosm biofilm model. Shear bond strength and adhesive remnant index were also tested. Biofilm activity precipitously dropped when contacting orthodontic cement with DMAHDM. Orthodontic cement containing 3% DMAHDM significantly reduced biofilm metabolic activity and lactic acid production (p<0.05), and decreased biofilm colony-forming unit (CFU) by two log. Water-aging for 90 days had no adverse influence on enamel shear bond strength (p>0.1). By incorporating DMAHDM into Transbond XT for the first time, the modified orthodontic cement obtained a strong antibacterial capability without compromising the enamel bond strength.

Objectives: White spot lesions due to biofilm acid-induced enamel demineralization are prevalent in orthodontic treatments. The aim of this study was to develop a novel bioactive multifunctional cement with protein-repellent, antibacterial and remineralizing capabilities, and investigate the effects on enamel hardness and lesion depth in vitro for the first time., Materials and Methods: 2-Methacryloyloxyethyl phosphorylcholine (MPC), dimethylaminohexadecyl methacrylate (DMAHDM), and nanoparticles of amorphous calcium phosphate (NACP) were incorporated into a resin-modified glass ionomer (RMGI). Extracted human premolars had brackets bonded via four groups: (1) Transbond XT (TB), (2) RMGI (GC Ortho LC), (3) RMGI+MPC+DMAHDM, (4) RMGI+MPC+DMAHDM+NACP. Demineralization was induced via a dental plaque microcosm biofilm model. Samples were tested using polarized light microscopy (PLM) for lesion depth. Enamel hardness was tested for different groups., Results: Incorporating MPC, DMAHDM and NACP did not affect enamel bond strength. "RMGI+MPC+DMAHDM+NACP" group had the least lesion depth in enamel (p<0.05). Groups with NACP had the highest enamel hardness (p<0.05). Mineral loss (ΔS) in enamel for NACP group was about one third that for RMGI control. "RMGI+MPC+DMAHDM" had greater effect on demineralization-inhibition, compared to RMGI and TB controls. "RMGI+MPC+DMAHDM+NACP" was more effective in protecting enamel prisms from dissolution by biofilm acids, compared to RMGI and TB control groups., Conclusion: The Novel "RMGI+MPC+DMAHDM+NACP" cement substantially reduced enamel demineralization adjacent to orthodontic brackets, yielding much less lesion depth and greater enamel hardness under biofilm acid attacks than commercial controls. The clinical significance is that the novel multi-agent (RMGI+MPC+DMAHDM+NACP) method is promising for a wide range of preventive and restorative applications to combat caries., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

Objective: A new adhesive containing nanoparticles of amorphous calcium phosphate (NACP) with calcium (Ca) and phosphate (P) ion rechargeability was recently developed; however, it was not antibacterial. The objectives of this study were to: (1) develop a novel adhesive with triple benefits of Ca and P ion recharge, protein-repellent and antibacterial functions via dimethylaminohexadecyl methacrylate (DMAHDM) and 2-methacryloyloxyethyl phosphorylcholine (MPC); and (2) investigate dentin bond strength, protein adsorption, Ca and P ion concentration, microcosm biofilm response and pH properties., Methods: MPC, DMAHDM and NACP were mixed into a resin consisting of ethoxylated bisphenol A dimethacrylate (EBPADMA), pyromellitic glycerol dimethacrylate (PMGDM), 2-hydroxyethyl methacrylate (HEMA) and bisphenol A glycidyl dimethacrylate (BisGMA). Protein adsorption was measured using a micro bicinchoninic acid method. A human saliva microcosm biofilm model was tested on resins. Colony-forming units (CFU), live/dead assay, metabolic activity, Ca and P ion concentration and biofilm culture medium pH were determined., Results: The adhesive with 5% MPC+5% DMAHDM+30% NACP inhibited biofilm growth, reducing biofilm CFU by 4 log, compared to control (p<0.05). Dentin shear bond strengths were similar (p>0.1). Biofilm medium became a Ca and P ion reservoir having ion concentration increasing with NACP filler level. The adhesive with 5% MPC+5% DMAHDM+30% NACP maintained a safe pH>6, while commercial adhesive had a cariogenic pH of 4., Significance: The new adhesive with triple benefits of Ca and P ion recharge, protein-repellent and antibacterial functions substantially reduced biofilm growth, reducing biofilm CFU by 4 orders of magnitude, and yielding a much higher pH than commercial adhesive. This novel adhesive is promising to protect tooth structures from biofilm acids. The method of using NACP, MPC and DMAHDM is promising for application to other dental materials to combat caries., (Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

White spot lesions (WSL) due to enamel demineralization are major complications for orthodontic treatments. Calcium phosphate (CaP) dental resins with Ca and P ion releases are promising for remineralization. However, previous Ca and P releases lasted for only weeks. Experimental orthodontic cements were developed using pyromellitic glycerol dimethacrylate (PMGDM) and ethoxylated bisphenol A dimethacrylate (EBPADMA) at mass ratio of 1:1 (PE); and PE plus 10% of 2-hydroxyethyl methacrylate (HEMA) and 5% of bisphenol A glycidyl dimethacrylate (BisGMA) (PEHB). Particles of amorphous calcium phosphate (ACP) were incorporated into PE and PEHB at 40% filler level. Specimens were tested for bracket-enamel shear bond strength, water sorption, CaP release, and ion recharge and re-release. PEHB+40ACP had higher bracket-enamel bond strength and ion release and rechargeability than PE+40ACP. ACP incorporation into the novel orthodontic cement did not adversely affect the bracket-enamel bond strength. Ion release and re-release from the novel ACP orthodontic cement indicated favorable release and re-release patterns. The recharged orthodontic cement could release CaP ions continuously for four weeks without further recharge. Novel rechargeable orthodontic cement containing ACP was developed with a high bracket-enamel bond strength and the ability to be repeatedly recharged to maintain long-term high levels of CaP ion releases., Competing Interests: The authors Xu H, Zhang L, Weir MD. declares the U.S. Provisional Patent Application. Number: 62/1121,438 (2015).

The objectives of this study were to: (1) develop a new bioactive dental bonding agent with nanoparticles of amorphous calcium phosphate and dimethylaminohexadecyl methacrylate for tooth root caries restorations and endodontic applications, and (2) investigate biofilm inhibition by the bioactive bonding agent against eight species of periodontal and endodontic pathogens for the first time. Bonding agent was formulated with 5 % of dimethylaminohexadecyl methacrylate. Nanoparticles of amorphous calcium phosphate at 30 wt% was mixed into adhesive. Eight species of biofilms were grown on resins: Porphyromonas gingivalis, Prevotella intermedia, Prevotella nigrescens, Aggregatibacter actinomycetemcomitans, Fusobacterium nucleatum, Parvimonas micra, Enterococcus faecalis, Enterococcus faecium. Colony-forming units, live/dead assay, biomass, metabolic activity and polysaccharide of biofilms were determined. The results showed that adding dimethylaminohexadecyl methacrylate and nanoparticles of amorphous calcium phosphate into bonding agent did not decrease dentin bond strength (P > 0.1). Adding dimethylaminohexadecyl methacrylate reduced the colony-forming units of all eight species of biofilms by nearly three orders of magnitude. The killing efficacy of dimethylaminohexadecyl methacrylate resin was: P. gingivalis > A. actinomycetemcomitans > P. intermedia > P. nigrescens > F. nucleatum > P. micra > E. faecalis > E. faecium. Dimethylaminohexadecyl methacrylate resin had much less biomass, metabolic activity and polysaccharide of biofilms than those without dimethylaminohexadecyl methacrylate (P < 0.05). In conclusion, a novel dental adhesive was developed for root caries and endodontic applications, showing potent inhibition of biofilms of eight species of periodontal and endodontic pathogens, and reducing colony-forming units by three orders of magnitude. The bioactive adhesive is promising for tooth root restorations to provide subgingival margins with anti-periodontal pathogen capabilities, and for endodontic sealer applications to combat endodontic biofilms.

Objectives: White spot lesions often occur in orthodontic treatments. The objective of this study was to develop a novel resin-modified glass ionomer cement (RMGI) as an orthodontic cement with protein-repellent, antibacterial and remineralization capabilities., Methods: Protein-repellent 2-methacryloyloxyethyl phosphorylcholine (MPC), antibacterial dimethylaminohexadecyl methacrylate (DMAHDM), nanoparticles of silver (NAg), and nanoparticles of amorphous calcium phosphate (NACP) were incorporated into a RMGI. Enamel shear bond strength (SBS) was determined. Calcium (Ca) and phosphate (P) ion releases were measured. Protein adsorption onto specimens was determined by a micro bicinchoninic acid method. A dental plaque microcosm biofilm model was tested., Results: Increasing the NACP filler level increased the Ca and P ion release. Decreasing the solution pH increased the ion release. Incorporating MPC into RMGI reduced protein adsorption, which was an order of magnitude less than that of commercial controls. Adding DMAHDM and NAg into RMGI yielded a strong antibacterial function, greatly reducing biofilm viability and acid production. Biofilm CFU counts on the multifunctional orthodontic cement were 3 orders of magnitude less than that of commercial control (p<0.05). These benefits were achieved without compromising the enamel shear bond strength (p>0.1)., Conclusions: A novel multifunctional orthodontic cement was developed with strong antibacterial and protein-repellent capabilities for preventing enamel demineralization., Clinical Significance: The new cement is promising to prevent white spot lesions in orthodontic treatments. The method of incorporating four bioactive agents may have wide applicability to the development of other bioactive dental materials to inhibit caries., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

The objectives of this study were to develop the first protein-repellent resin-modified glass ionomer cement (RMGI) by incorporating 2-methacryloyloxyethyl phosphorylcholine (MPC) for orthodontic applications, and to investigate the MPC effects on protein adsorption, biofilm growth, and enamel bond strength. MPC was incorporated into RMGI at 0% (control), 1.5%, 3%, and 5% by mass. Specimens were stored in water at 37°C for 1 and 30 days. Enamel shear bond strength (SBS) was measured, and the adhesive remnant index (ARI) scores were assessed. Protein adsorption onto the specimens was determined by a micro bicinchoninic acid method. A dental plaque microcosm biofilm model with human saliva as inoculum was used. The results showed that adding 3% of MPC into RMGI did not significantly reduce the SBS (p > 0.1). There was no significant loss in SBS for RMGI containing 3% MPC after water-aging for 30 days, as compared to 1 day (p > 0.1). RMGI with 3% MPC had protein adsorption that was 1/10 that of control. RMGI with 3% MPC greatly reduced the bacterial adhesion, and lactic acid production and colony-forming units of biofilms, while substantially increasing the medium solution pH containing biofilms. The protein-repellent and biofilm-repellent effects were not decreased after water-aging for 30 days. In conclusion, the MPC-containing RMGI is promising to reduce biofilms and white spot lesions without compromising orthodontic bracket-enamel bond strength. The novel protein-repellent method may have applicability to other orthodontic cements, dental composites, adhesives, sealants, and cements to repel proteins and biofilms. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 104B: 949-959, 2016., (© 2015 Wiley Periodicals, Inc.)

Objectives: White spot lesions are the most undesired side-effect of fixed orthodontic treatments. The objectives of this study were to combine nanoparticles of silver (NAg) with 2-methacryloyloxyethyl phosphorylcholine (MPC) to develop a modified resin-modified glass ionomer cement (RMGI) as orthodontic cement with double benefits of antibacterial and protein-repellent capabilities for the first time., Methods: NAg and MPC were incorporated into a commercial RMGI. Another commercial orthodontic adhesive also served as control. Enamel shear bond strengths (SBS) were determined. Protein adsorption was measured via a micro bicinchoninic acid method. A dental plaque microcosm biofilm model with human saliva as inoculum was tested. Biofilms adherent on the cement samples and planktonic bacteria in the culture medium away from the cement surfaces were both evaluated for bacterial metabolic activity, colony-forming units (CFU), and lactic acid production., Results: Adding 0.1% NAg and 3% MPC to RMGI, and water-aging for 30 days, did not adversely affect the SBS, compared to the unmodified RMGI control (p>0.1). The modified RMGI containing 0.1% NAg and 3% MPC achieved the greatest reduction in protein adsorption, bacterial adhesion, CFU, metabolic activity and lactic acid production. The RMGI containing 0.1% NAg and 3% MPC inhibited not only the bacteria on its surface, but also the bacteria away from the surface in the culture medium., Conclusions: The incorporation of double agents (antibacterial NAg+protein-repellent MPC) into RMGI achieved much stronger inhibition of biofilms than using each agent alone. The novel antibacterial and protein-repellent RMGI with substantially-reduced biofilm acids is promising as an orthodontic cement to combat white spot lesions in enamel., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Objectives: The tooth-resin bond is the weak link of restoration, with secondary caries as a main reason for failure. Calcium phosphate-containing resins are promising for remineralization; however, calcium (Ca) and phosphate (P) ion releases last only a couple of months. The objectives of this study were to develop the first rechargeable CaP bonding agent and investigate the key factors that determine CaP ion recharge and re-release., Methods: Nanoparticles of amorphous calcium phosphate (NACP) were synthesized. Pyromellitic glycerol dimethacrylate (PMGDM), ethoxylated bisphenol-A dimethacrylate (EBPADMA), 2-hydroxyethyl methacrylate (HEMA), and bisphenol-A glycidyl dimethacrylate (BisGMA) were used to synthesize three adhesives (denoted PE, PEH and PEHB). NACP were mixed into adhesive at 0-30% by mass. Dentin shear bond strengths were measured. Adhesive specimens were tested for Ca and P initial ion release. Then the ion-exhausted specimens were immersed in Ca and P solution to recharge the specimens, and the recharged specimens were then used to measure ion re-release for 7 days as one cycle. Then these specimens were again recharged and the re-release was measured for 7 days as the second cycle. Three recharge/re-release cycles were tested., Results: PEHB had the highest dentin bond strength (p<0.05). Increasing NACP content from 0 to 30% did not affect dentin bond strength (p>0.1), but increased CaP release and re-release (p<0.05). PEHB-NACP had the greatest recharge/re-release, and PE-NACP had the least (p<0.05). Ion release remained high and did not decrease with increasing the number of recharge/re-release cycles (p>0.1). After the third cycle, specimens without further recharge had continuous CaP ion release for 2-3 weeks., Significance: Rechargeable CaP bonding agents were developed for the first time to provide long-term Ca and P ions to promote remineralization and reduce caries. Incorporation of NACP into adhesive had no negative effect on dentin bond strength. Increasing NACP filler level increased the ion recharge and re-release capability. The new CaP recharge method and PMGDM-EBPADMA-NACP composition may have wide application in adhesives, composites and cements, to combat caries and remineralize lesions., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Objectives: The objectives of this study were to: (1) develop a novel adhesive for prevention of tooth root caries and secondary caries by possessing a combination of protein-repellent, antibacterial, and remineralization capabilities for the first time; and (2) investigate the effects of 2-methacryloyloxyethyl phosphorylcholine (MPC), dimethylaminohexadecyl methacrylate (DMAHDM), and nanoparticles of amorphous calcium phosphate (NACP) on dentin bond strength, protein-repellent properties, and dental plaque microcosm biofilm response., Methods: MPC, DMAHDM and NACP were added into Scotchbond Multi-Purpose primer and adhesive. Dentin shear bond strengths were measured. Adhesive coating thickness, surface texture and dentin-adhesive interfacial structure were examined. Protein adsorption onto adhesive resin surface was determined by the micro bicinchoninic acid method. A human saliva microcosm biofilm model was used to investigate biofilm metabolic activity, colony-forming unit (CFU) counts, and lactic acid production., Results: The resin with 7.5% MPC+5% DMAHDM+30% NACP did not adversely affect dentin shear bond strength (p>0.1). The resin with 7.5% MPC+5% DMAHDM+30% NACP produced a coating on root dentin with a thickness of approximately 70μm and completely sealed all the dentinal tubules. The resin with 7.5% MPC+5% DMAHDM+30% NACP had 95% reduction in protein adsorption, compared to SBMP control (p<0.05). The resin with 7.5% MPC+5% DMAHDM+30% NACP was strongly antibacterial, with biofilm CFU being four orders of magnitude lower than that of SBMP control. Significance The novel multifunctional adhesive with strong protein-repellent, antibacterial and remineralization properties is promising to coat tooth roots to prevent root caries and secondary caries. The combined use of MPC, DMAHDM and NACP may have wide applicability to bonding agents, cements, sealants and composites to inhibit caries., (Copyright © 2015 Academy of Dental Materials. All rights reserved.)

Objectives: Secondary caries at the tooth-restoration margins remains a main reason for restoration failure. The objectives of this study were to: (1) combine protein-repellent 2-methacryloyloxyethyl phosphorylcholine (MPC) with quaternary ammonium dimethylaminohexadecyl methacrylate (DMAHDM) to develop a new dental adhesive with double benefits of protein-repellent and antibacterial capabilities for the first time; and (2) investigate the effects on protein adsorption, anti-biofilm activity, and dentin bond strength., Methods: MPC and DMAHDM were incorporated into Scotchbond Multi-Purpose (SBMP) primer and adhesive. Dentin shear bond strengths were measured using extracted human molars. Protein adsorption onto the adhesive resin surfaces was determined by the micro bicinchoninic acid (BCA) method. A dental plaque microcosm biofilm model with human saliva as inoculum was used to investigate biofilm metabolic activity, colony-forming unit (CFU) counts, lactic acid production and live/dead staining of biofilms on resins., Results: Incorporation of 7.5% MPC and 5% DMAHDM into primer and adhesive did not adversely affect the dentin shear bond strength (p>0.1). The resin with 7.5% MPC+5% DMAHDM had protein adsorption that was nearly 20-fold less than SBMP control (p<0.05). The resin with 7.5% MPC+5% DMAHDM had much stronger antibacterial effects than using MPC or DMAHDM alone (p<0.05). Biofilm CFU counts on the resin with 7.5% MPC+5% DMAHDM were reduced by more than 4 orders of magnitude, compared to SBMP control., Significance: The use of double agents (protein-repellent MPC+antibacterial DMAHDM) in dental adhesive achieved much stronger inhibition of biofilms than using each agent alone. The novel protein-repellent and antibacterial bonding agent is promising to reduce biofilm/plaque buildup and reduce recurrent caries at the tooth-restoration margins., (Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

Antibacterial bonding agents and composites containing dimethylaminododecyl methacrylate (DMADDM) have been recently developed. The objectives of this study were to investigate the antibacterial effect of novel adhesives containing different mass fractions of DMADDM on Streptococcus mutans (S. mutans) biofilm at different developmental stages. Different mass fractions of DMADDM were incorporated into adhesives and S. mutans biofilm at different developmetal stages were analyzed by MTT assays, lactic acid measurement, confocal laser scanning microscopy and scanning electron microscopy observations. Exopolysaccharides (EPS) staining was used to analyze the inhibitory effect of DMADDM on the biofilm extracellular matrix. Dentin microtensile strengths were also measured. Cured adhesives containing DMADDM could greatly reduce metabolic activity and lactic acid production during the development of S. mutans biofilms (p < 0.05). In earlier stages of biofilm development, there were no significant differences of inhibitory effects between the 2.5% DMADDM and 5% DMADDM group. However, after 72 h, the anti-biofilm effects of adhesives containing 5% DMADDM were significantly stronger than any other group. Incorporation of DMADDM into adhesive did not adversely affect dentin bond strength. In conclusion, adhesives containing DMADDM inhibited the growth, lactic acid production and EPS metabolism of S. mutans biofilm at different stages, with no adverse effect on its dentin adhesive bond strength. The bonding agents have the potential to control dental biofilms and combat tooth decay, and DMADDM is promising for use in a wide range of dental adhesive systems and restoratives.

Objectives: Calcium phosphate cement (CPC) is promising for dental and craniofacial applications due to its ability to be injected or filled into complex-shaped bone defects and molded for esthetics, and its resorbability and replacement by new bone. The objective of this study was to investigate bone regeneration via novel macroporous CPC containing absorbable fibers, hydrogel microbeads and growth factors in critical-sized cranial defects in rats., Methods: Mannitol porogen and alginate hydrogel microbeads were incorporated into CPC. Absorbable fibers were used to provide mechanical reinforcement to CPC scaffolds. Six CPC groups were tested in rats: (1) control CPC without macropores and microbeads; (2) macroporous CPC+large fiber; (3) macroporous CPC+large fiber+nanofiber; (4) same as (3), but with rhBMP2 in CPC matrix; (5) same as (3), but with rhBMP2 in CPC matrix+rhTGF-β1 in microbeads; (6) same as (3), but with rhBMP2 in CPC matrix+VEGF in microbeads. Rats were sacrificed at 4 and 24 weeks for histological and micro-CT analyses., Results: The macroporous CPC scaffolds containing porogen, absorbable fibers and hydrogel microbeads had mechanical properties similar to cancellous bone. At 4 weeks, the new bone area fraction (mean±sd; n=5) in CPC control group was the lowest at (14.8±3.3)%, and that of group 6 (rhBMP2+VEGF) was (31.0±13.8)% (p<0.05). At 24 weeks, group 4 (rhBMP2) had the most new bone of (38.8±15.6)%, higher than (12.7±5.3)% of CPC control (p<0.05). Micro-CT revealed nearly complete bridging of the critical-sized defects with new bone for several macroporous CPC groups, compared to much less new bone formation for CPC control., Significance: Macroporous CPC scaffolds containing porogen, fibers and microbeads with growth factors were investigated in rat cranial defects for the first time. Macroporous CPCs had new bone up to 2-fold that of traditional CPC control at 4 weeks, and 3-fold that of traditional CPC at 24 weeks, and hence may be useful for dental, craniofacial and orthopedic applications., (Copyright © 2014 Academy of Dental Materials. All rights reserved.)

Antibacterial and remineralizing dental composites and adhesives were recently developed to inhibit biofilm acids and combat secondary caries. It is not clear what effect these materials will have on dental pulps in vivo. The objectives of this study were to investigate the antibacterial and remineralizing restorations in a rat tooth cavity model, and determine pulpal inflammatory response and tertiary dentin formation. Nanoparticles of amorphous calcium phosphate (NACP) and antibacterial dimethylaminododecyl methacrylate (DMADDM) were synthesized and incorporated into a composite and an adhesive. Occlusal cavities were prepared in the first molars of rats and restored with four types of restoration: control composite and adhesive; control plus DMADDM; control plus NACP; and control plus both DMADDM and NACP. At 8 or 30days, rat molars were harvested for histological analysis. For inflammatory cell response, regardless of time periods, the NACP group and the DMADDM+NACP group showed lower scores (better biocompatibility) than the control group (p=0.014 for 8days, p=0.018 for 30days). For tissue disorganization, NACP and DMADDM+NACP had better scores than the control (p=0.027) at 30days. At 8days, restorations containing NACP had a tertiary dentin thickness (TDT) that was five- to six-fold that of the control. At 30days, restorations containing NACP had a TDT that was four- to six-fold that of the control. In conclusion, novel antibacterial and remineralizing restorations were tested in rat teeth in vivo for the first time. Composite and adhesive containing NACP and DMADDM exhibited milder pulpal inflammation and much greater tertiary dentin formation than the control adhesive and composite. Therefore, the novel composite and adhesive containing NACP and DMADDM are promising as a new therapeutic restorative system to not only combat oral pathogens and biofilm acids as shown previously, but also facilitate the healing of the dentin-pulp complex., (Published by Elsevier Ltd.)

Objectives: Calcium phosphate cement (CPC) is promising for dental and craniofacial repairs. Vascularization in bone tissue engineering constructs is currently a major challenge. The objectives of this study were to investigate the prevascularization of macroporous CPC via coculturing human umbilical vein endothelial cells (HUVEC) and human osteoblasts (HOB), and determine the effect of RGD in CPC on microcapillary formation for the first time., Methods: Macroporous CPC scaffold was prepared using CPC powder, chitosan liquid and gas-foaming porogen. Chitosan was grafted with Arg-Gly-Asp (RGD) to biofunctionalize the CPC. HUVEC and HOB were cocultured on macroporous CPC-RGD and CPC control without RGD for up to 42d. The osteogenic and angiogenic differentiation, bone matrix mineral synthesis, and formation of microcapillary-like structures were measured., Results: RGD-grafting in CPC increased the gene expressions of osteogenic and angiogenic differentiation markers than those of CPC control without RGD. Cell-synthesized bone mineral content also increased on CPC-RGD, compared to CPC control (p<0.05). Immunostaining with endothelial marker showed that the amount of microcapillary-like structures on CPC scaffolds increased with time. At 42d, the cumulative vessel length for CPC-RGD scaffold was 1.69-fold that of CPC control. SEM examination confirmed the morphology of self-assembled microcapillary-like structures on CPC scaffolds., Significance: HUVEC+HOB coculture on macroporous CPC scaffold successfully achieved prevascularization. RGD incorporation in CPC enhanced osteogenic differentiation, bone mineral synthesis, and microcapillary-like structure formation. The novel prevascularized CPC-RGD constructs are promising for dental, craniofacial and orthopedic applications., (Copyright © 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

Objectives: Antibacterial primer and adhesive are promising to inhibit biofilms and caries. Since restorations in vivo are exposed to saliva, one concern is the attenuation of antibacterial activity due to salivary pellicles. The objective of this study was to investigate the effects of salivary pellicles on bonding agents containing a new monomer dimethylaminododecyl methacrylate (DMADDM) or nanoparticles of silver (NAg) against biofilms for the first time., Methods: DMADDM and NAg were synthesized and incorporated into Scotchbond Multi-Purpose adhesive and primer. Specimens were either coated or not coated with salivary pellicles. A microcosm biofilm model was used with mixed saliva from ten donors. Two types of culture medium were used: an artificial saliva medium (McBain), and Brain Heart Infusion (BHI) medium without salivary proteins. Metabolic activity, colony-forming units (CFU), and lactic acid production of plaque microcosm biofilms were measured (n=6)., Results: Bonding agents containing DMADDM and NAg greatly inhibited biofilm activities, even with salivary pellicles. When using BHI, the pre-coating of salivary pellicles on resin surfaces significantly decreased the antibacterial effect (p<0.05). When using artificial saliva medium, pre-coating of salivary pellicles on resin did not decrease the antibacterial effect. These results suggest that artificial saliva yielded medium-derived pellicles on resin surfaces, which provided attenuating effects on biofilms similar to salivary pellicles. Compared with the commercial control, the DMADDM-containing bonding agent reduced biofilm CFU by about two orders of magnitude., Significance: Novel DMADDM- and NAg-containing bonding agents substantially reduced biofilm growth even with salivary pellicle coating on surfaces, indicating a promising usage in saliva-rich environment. DMADDM and NAg may be useful in a wide range of primers, adhesives and other restoratives to achieve antibacterial and anti-caries capabilities., (Published by Elsevier Ltd.)

Objectives: Many recent adhesives on the market exhibit reasonable clinical performance. Future innovations in adhesive materials should therefore seek out novel properties rather than simply modifying existing technologies. It is proposed that adhesive materials that are "bio-active" could contribute to better prognosis of restorative treatments., Methods: This review examines the recent approaches used to achieve therapeutic polymers for dental adhesives by incorporating bio-active components. A strategy to maintain adhesive restorations is the focus of this paper., Results: Major trials on therapeutic dental adhesives have looked at adding antibacterial activities or remineralization effects. Applications of antibacterial resin monomers based on quaternary ammonium compounds have received much research attention, and the loading of nano-sized bioactive particles or multiple ion-releasing glass fillers have been perceived as advantageous since they are not expected to influence the mechanical properties of the carrier polymer., Significance: The therapeutic polymer approaches described here have the potential to provide clinical benefits. However, not many technological applications in this category have been successfully commercialized. Clinical evidence as well as further advancement of these technologies can be a driving force to make these new types of materials clinically available., (Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

Dental resins containing 12-methacryloyloxydodecylpyridinium bromide (MDPB) showed potent antibacterial functions. Recent studies developed antibacterial resins containing nanoparticles of silver (NAg). The objectives of this study were to develop an adhesive containing dual agents of MDPB and NAg for the first time and to investigate the combined effects of antibacterial adhesive and primer on biofilm viability, metabolic activity, lactic acid, dentin bond strength, and fibroblast cytotoxicity. MDPB and NAg were incorporated into Scotchbond Multi-Purpose (SBMP) adhesive "A" and primer "P". Five systems were tested: SBMP adhesive A; A + MDPB; A+NAg; A + MDPB + NAg; P + MDPB + NAg together with A + MDPB + NAg. Dental plaque microcosm biofilms were cultured using mixed saliva from 10 donors. Metabolic activity, colony-forming units, and lactic acid production of biofilms were investigated. Human fibroblast cytotoxicity of bonding agents was determined. MDPB + NAg in adhesive/primer did not compromise dentin bond strength (p > 0.1). MDPB or NAg alone in adhesive substantially reduced the biofilm activities. Dual agents MDPB + NAg in adhesive significantly reduced the biofilm viability compared with each agent alone (p < 0.05). The greatest inhibition of biofilms was achieved when both adhesive and primer contained MDPB + NAg. Fibroblast viability of groups with dual antibacterial agents was similar to control using culture medium without resin eluents (p > 0.1). In conclusion, this study showed for the first time that the antibacterial potency of MDPB adhesive could be substantially enhanced via NAg. Adding MDPB + NAg into both primer and adhesive achieved the strongest antibiofilm efficacy. The dual agent (MDPB + NAg) method could have wide applicability to other adhesives, sealants, cements, and composites to inhibit biofilms and caries., (Copyright © 2013 Wiley Periodicals, Inc.)

Secondary caries remains the main reason for dental restoration failure. Replacement of failed restorations accounts for 50%-70% of all restorations performed. Antibacterial adhesives could inhibit biofilm acids at tooth-restoration margins, and calcium phosphate (CaP) ions could remineralize tooth lesions. The objectives of this study were to: (1) incorporate nanoparticles of silver (NAg), quaternary ammonium dimethacrylate (QADM), and nanoparticles of amorphous calcium phosphate (NACP) into bonding agent; and (2) investigate their effects on dentin bonding and microcosm biofilms. An experimental primer was made with pyromellitic glycerol dimethacrylate (PMGDM) and 2-hydroxyethyl methacrylate (HEMA). An adhesive was made with bisphenol-A-glycerolate dimethacrylate (BisGMA) and triethylene glycol dimethacrylate (TEGDMA). NAg was incorporated into primer at 0.1 wt %. The adhesive contained 0.1% NAg and 10% QADM, and 0%-40% NACP. Incorporating NAg into primer and NAg-QADM-NACP into adhesive did not adversely affect dentin bond strength (p > 0.1). Scanning electron microscopy showed numerous resin tags, and transmission electron microscopy revealed NAg and NACP in dentinal tubules. Viability of human saliva microcosm biofilms on primer/adhesive/composite disks was substantially reduced via NAg and QADM. Metabolic activity, lactic acid, and colony-forming units of biofilms were much lower on the new bonding agents than control (p < 0.05). In conclusion, novel dental bonding agents containing NAg, QADM, and NACP were developed with the potential to kill residual bacteria in the tooth cavity and inhibit the invading bacteria along tooth-restoration margins, with NACP to remineralize tooth lesions. The novel method of combining antibacterial agents (NAg and QADM) with remineralizing agent (NACP) may have wide applicability to other adhesives for caries inhibition., (Copyright © 2012 Wiley Periodicals, Inc.)

Objective: Antibacterial primer and adhesive are promising to help combat biofilms and recurrent caries. The objectives of this study were to compare novel bonding agent containing quaternary ammonium dimethacrylate (QADM) with bonding agent containing nanoparticles of silver (NAg) in antibacterial activity, contact-inhibition vs. long-distance inhibition, glucosyltransferases (gtf) gene expressions, and cytotoxicity for the first time., Methods: QADM and NAg were incorporated into Scotchbond Multi-Purpose adhesive and primer. Microtensile dentin bond strength was measured. Streptococcus mutans (S. mutans) biofilm on resin surface (contact-inhibition) as well as S. mutans in culture medium away from the resin surface (long-distance inhibition) were tested for metabolic activity, colony-forming units (CFUs), lactic acid production, and gtf gene expressions. Eluents from cured primer/adhesive samples were used to examine cytotoxicity against human gingival fibroblasts., Results: Bonding agent with QADM greatly reduced CFU and lactic acid of biofilms on the resin surface (p<0.05), while having no effect on S. mutans in culture medium away from the resin surface. In contrast, bonding agent with NAg inhibited not only S. mutans on the resin surface, but also S. mutans in culture medium away from the resin surface. Bonding agent with QADM suppressed gtfB, gtfC and gtfD gene expressions of S. mutans on its surface, but not away from its surface. Bonding agent with NAg suppressed S. mutans gene expressions both on its surface and away from its surface. Bonding agents with QADM and NAg did not adversely affect microtensile bond strength or fibroblast cytotoxicity, compared to control (p>0.1)., Significance: QADM-containing adhesive had contact-inhibition and inhibited bacteria on its surface, but not away from its surface. NAg-containing adhesive had long-distance killing capability and inhibited bacteria on its surface and away from its surface. The novel antibacterial adhesives are promising for caries-inhibition restorations, and QADM and NAg could be complimentary agents in inhibiting bacteria on resin surface as well as away from resin surface., (Published by Elsevier Ltd.)

Objectives: The main reason for restoration failure is secondary caries caused by biofilm acids. Replacing the failed restorations accounts for 50-70% of all operative work. The objectives of this study were to incorporate a new quaternary ammonium monomer (dimethylaminododecyl methacrylate, DMADDM) and nanoparticles of silver (NAg) into a primer and an adhesive, and to investigate their effects on antibacterial and dentin bonding properties., Methods: Scotchbond Multi-Purpose (SBMP) served as control. DMADDM was synthesized and incorporated with NAg into primer/adhesive. A dental plaque microcosm biofilm model with human saliva was used to investigate metabolic activity, colony-forming units (CFU), and lactic acid. Dentin shear bond strengths were measured., Results: Minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of the new DMADDM were orders of magnitude lower than those of a previous quaternary ammonium dimethacrylate (QADM). Uncured primer with DMADDM had much larger inhibition zones than QADM (p<0.05). Cured primer/adhesive with DMADDM-NAg greatly reduced biofilm metabolic activity (p<0.05). Combining DMADDM with NAg in primer/adhesive resulted in less CFU than DMADDM alone (p<0.05). Lactic acid production by biofilms was reduced by 20-fold via DMADDM-NAg, compared to control. Incorporation of DMADDM and NAg into primer/adhesive did not adversely affect dentin bond strength., Conclusions: A new antibacterial monomer DMADDM was synthesized and incorporated into primer/adhesive for the first time. The bonding agents are promising to combat residual bacteria in tooth cavity and invading bacteria at tooth-restoration margins to inhibit caries. DMADDM and NAg are promising for use into a wide range of dental adhesive systems and restoratives., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Objectives: Secondary caries is the main reason for restoration failure, and replacement of the failed restorations accounts for 50-70% of all restorations. Antibacterial adhesives could inhibit residual bacteria in tooth cavity and invading bacteria along the margins. Calcium (Ca) and phosphate (P) ion release could remineralize the lesions. The objectives of this study were to incorporate nanoparticles of silver (NAg) and nanoparticles of amorphous calcium phosphate (NACP) into adhesive for the first time, and to investigate the effects on dentin bond strength and plaque microcosm biofilms., Methods: Scotchbond multi-purpose adhesive was used as control. NAg were added into primer and adhesive at 0.1% by mass. NACP were mixed into adhesive at 10%, 20%, 30% and 40%. Microcosm biofilms were grown on disks with primer covering the adhesive on a composite. Biofilm metabolic activity, colony-forming units (CFU) and lactic acid were measured., Results: Human dentin shear bond strengths (n=10) ranged from 26 to 34 MPa; adding NAg and NACP into adhesive did not decrease the bond strength (p>0.1). SEM examination revealed resin tags from well-filled dentinal tubules. Numerous NACP infiltrated into the dentinal tubules. While NACP had little antibacterial effect, NAg in bonding agents greatly reduced the biofilm viability and metabolic activity, compared to the control (p<0.05). CFU for total microorganisms, total streptococci, and mutans streptococci on bonding agents with NAg were an order of magnitude less than those of the control. Lactic acid production by biofilms for groups containing NAg was 1/4 of that of the control., Significance: Dental plaque microcosm biofilm viability and acid production were greatly reduced on bonding agents containing NAg and NACP, without compromising dentin bond strength. The novel method of incorporating dual agents (remineralizing agent NACP and antibacterial agent NAg) may have wide applicability to other dental bonding systems., (Copyright © 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

Dental composites do not hinder bacteria colonization and plaque formation. Caries at the restoration margins is a frequent reason for replacement of existing restorations, which accounts for 50 to 70% of all restorations. The objectives of this study were to examine the filler level effect on nanocomposite containing nanoparticles of amorphous calcium phosphate (NACP) and investigate the load-bearing and acid-neutralizing properties and bacteria inhibition. NACP with 116-nm particle size were synthesized via a spray-drying technique and incorporated into a resin. Flexural strength of nanocomposite with 10 to 30% NACP fillers matched the strength of a commercial hybrid composite (p > 0.1). Nanocomposite with 40% NACP matched the strength of a microfill composite, which was 2-fold that of a resin-modified glass ionomer. Nanocomposite with 40% NACP neutralized a lactic acid solution of pH 4 by rapidly increasing the pH to 5.69 in 10 min. In contrast, the commercial controls had pH staying at near 4. Using Streptoccocus mutans, an agar disk-diffusion test showed no inhibition zone for commercial controls. In contrast, the inhibition zone was (2.5 ± 0.7) mm for nanocomposite with 40% NACP. Crystal violet staining showed that S. mutans coverage on nanocomposite was 1/4 that on commercial composite. In conclusion, novel calcium-phosphate nanocomposite matched the mechanical properties of commercial composite and rapidly neutralized lactic acid of pH 4. The nanocomposite appeared to moderately reduce the S. mutans growth, and further study is needed to obtain strong antimicrobial properties. The new nanocomposite may have potential to reduce secondary caries and restoration fracture, two main challenges facing tooth cavity restorations., (Copyright © 2011 Wiley Periodicals, Inc.)

Objectives: Calcium phosphate cement (CPC) is a promising material for dental, periodontal, and craniofacial repairs. However, its use requires on-site powder-liquid mixing that increases the surgical placement time and raises concerns of insufficient and inhomogeneous mixing. The objective of this study was to determine a formulation of premixed CPC (PCPC) with rapid setting, high strength, and good in vitro cell viability., Methods: PCPCs were formulated from CPC powder+non-aqueous liquid+gelling agent+hardening accelerator. Five PCPCs were thus developed: PCPC-Tartaric, PCPC-Malonic, PCPC-Citric, PCPC-Glycolic, and PCPC-Malic. Formulations and controls were compared for setting time, diametral tensile strength, and osteoblast cell compatibility., Results: Setting time (mean+/-S.D.; n=4) for PCPC-Tartaric was 8.2+/-0.8 min, significantly less than the 61.7+/-1.5 min for the Premixed Control developed previously (p<0.001). On 7th day immersion, the diametral tensile strength of PCPC-Tartaric reached 6.5+/-0.8 MPa, higher than 4.5+/-0.8 MPa of Premixed Control (p=0.036). Osteoblast cells displayed a polygonal morphology and attached to the nano-hydroxyapatite crystals in the PCPCs. All cements had similar live cell density values (p=0.126), indicating that the new PCPCs were as cell compatible as a non-premixed CPC control known to be biocompatible. Each of the new PCPCs had a cell viability that was not significantly different (p>0.1) from that of the non-premixed CPC control., Significance: PCPCs will eliminate the powder-liquid mixing during surgery and may also improve the cement performance. The new PCPCs supported cell attachment and yielded a high cell density and viability. Their mechanical strengths approached the reported strengths of sintered porous hydroxyapatite implants and cancellous bone. These nano-crystalline hydroxyapatite cements may be useful in dental, periodontal, and craniofacial repairs.

Self-hardening calcium phosphate cement (CPC) sets to form hydroxyapatite with high osteoconductivity, but its brittleness and low strength limit its use to only non-stress bearing locations. Previous studies developed bioactive composites containing hydroxyapatite fillers in Bis-GMA-based composites for bone repair applications, and they possessed higher strength values. However, these strengths were still lower than the strength of cortical bone. The aim of this study was to develop strong and bioactive composites by combining CPC fillers with nano-silica-fused whiskers in a resin matrix, and to characterize the mechanical properties and cell response. Silica particles were fused to silicon carbide whiskers to roughen the whisker surfaces for enhanced retention in the matrix. Mass ratios of whisker:CPC of 1:2, 1:1 and 2:1 were incorporated into a Bis-GMA-based resin and hardened by two-part chemical curing. Composite with only CPC fillers without whiskers served as a control. The specimens were tested using three-point flexure and nano-indentation. Composites with whisker:CPC ratios of 2:1 and 1:1 had flexural strengths (mean+/-SD; n=9) of (164+/-14) MPa and (139+/-22) MPa, respectively, nearly 3 times higher than (54+/-5) MPa of the control containing only CPC fillers (p<0.05). The strength of the new whisker-CPC composites was 3 times higher than the strength achieved in previous studies for conventional bioactive composites containing hydroxyapatite particles in Bis-GMA-based resins. The mechanical properties of the CPC-whisker composites nearly matched those of cortical bone and trabecular bone. Osteoblast-like cell adhesion, proliferation and viability were equivalent on the non-whisker control containing only CPC fillers, on the whisker composite at whisker:CPC of 1:1, and on the tissue culture polystyrene control, suggesting that the new CPC-whisker composite was non-cytotoxic.

Calcium phosphate cement (CPC) sets to form hydroxyapatite and has been used in medical and dental procedures. However, the brittleness and low strength of CPC prohibit its use in many stress-bearing locations, unsupported defects, or reconstruction of thin bones. Recent studies incorporated fibers into CPC to improve its strength. In the present study, a novel methodology was used to combine the reinforcement with macroporosity: large-diameter resorbable fibers were incorporated into CPC to provide short-term strength, then dissolved to create macropores suitable for bone ingrowth. Two types of resorbable fibers with 322 microm diameters were mixed with CPC to a fiber volume fraction of 25%. The set specimens were immersed in saline at 37 degrees C for 1, 7, 14, 28 and 56d, and were then tested in three-point flexure. SEM was used to examine crack-fiber interactions. CPC composite achieved a flexural strength 3 times, and work-of-fracture (toughness) nearly 100 times, greater than unreinforced CPC. The strength and toughness were maintained for 2-4 weeks of immersion, depending on fiber dissolution rate. Macropores or channels were observed in CPC composite after fiber dissolution. In conclusion, incorporating large-diameter resorbable fibers can achieve the needed short-term strength and fracture resistance for CPC while tissue regeneration is occurring, then create macropores suitable for vascular ingrowth when the fibers are dissolved. The reinforcement mechanisms appeared to be crack bridging and fiber pullout, the mechanical properties of the CPC matrix also affected the composite properties.

Orthodontic treatment is increasingly popular as people worldwide seek esthetics and better quality of life. In orthodontic treatment, complex appliances and retainers are placed in the patients' mouths for at least one year, which often lead to biofilm plaque accumulation. This in turn increases the caries-inducing bacteria, decreases the pH of the retained plaque on an enamel surface, and causes white spot lesions (WSLs) in enamel. This article reviews the cutting-edge research on a new class of bioactive and therapeutic dental resins, cements, and adhesives that can inhibit biofilms and protect tooth structures. The novel approaches include the use of protein-repellent and anticaries polymeric dental cements containing 2-methacryloyloxyethyl phosphorylcholine (MPC) and dimethylaminododecyl methacrylate (DMAHDM); multifunctional resins that can inhibit enamel demineralization; protein-repellent and self-etching adhesives to greatly reduce oral biofilm growth; and novel polymethyl methacrylate resins to suppress oral biofilms and acid production. These new materials could reduce biofilm attachment, raise local biofilm pH, and facilitate the remineralization to protect the teeth. This novel class of dental resin with dual benefits of antibacterial and protein-repellent capabilities has the potential for a wide range of dental and biomedical applications to inhibit bacterial infection and protect the tissues. [ABSTRACT FROM AUTHOR]

The objectives were to develop a novel rechargeable cement containing amorphous calcium-phosphate nanoparticles (nanoACP) to suppress tooth decay. Five cements were made with: (1) 60% glass particles (experimental control); (2) 40% glass+20% nanoACP; (3) 30% glass+30% nanoACP; (4) 20% glass+40% nanoACP; (5) 10% glass+50% nanoACP. Groups 1-4 had enamel bond strengths similar to Transbond XT (3M) and Vitremer (3M) (p>0.1). The nanoACP cement had calcium and phosphate ion release which increased with increasing nanoACP fillers. The recharged cement had substantial ion re-release continuously for 14 days after a single recharge. Ion re-release did not decrease with increasing recharge/re-release cycles. Groups 3-5 maintained a safe pH of medium (>5.5); however, control cements had cariogenic pH of medium (<4.5) due to biofilm acid. Therefore, nanoACP cement (1) had good bond strength to enamel, (2) possessed calcium and phosphate ion recharge/re-release capability, and (3) raised biofilm pH to a safe level to inhibit caries. [ABSTRACT FROM AUTHOR]