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1.
Dent Mater ; 40(7): 1025-1030, 2024 Jul.
Article in English | MEDLINE | ID: mdl-38755042

ABSTRACT

OBJECTIVES: Resin composites may release bisphenol A (BPA) due to impurities present in the monomers. However, there is a lack of knowledge regarding the leaching characteristics of BPA from resin composites. Therefore, experimental resin composites were prepared with known amounts of BPA. The objective of this study was (1) to determine which amount of BPA initially present in the material leaches out in the short term and, (2) how this release is influenced by the resin composition. METHODS: BPA (0, 0.001, 0.01, or 0.1 wt%) was added to experimental resin composites containing 60 mol% BisGMA, BisEMA(3), or UDMA, respectively, as base monomer and 40 mol% TEGDMA as diluent monomer. Polymerized samples (n = 5) were immersed at 37 °C for 7 days in 1 mL of water, which was collected and refreshed daily. BPA release was quantified with UPLC-MS/MS after derivatization with pyridine-3-sulfonyl chloride. RESULTS: Between 0.47 to 0.67 mol% of the originally added BPA eluted from the resin composites after 7 days. Similar elution trends were observed irrespective of the base monomer. Two-way ANOVA showed a significant effect of the base monomer on BPA release, but the differences were small and not consistent. SIGNIFICANCE: The released amount of BPA was directly proportional to the quantity of BPA present in the resin composite as an impurity. BPA release was mainly diffusion-based, while polymer composition seemed to play a minor role. Our results underscore the importance for manufacturers only to use monomers of the highest purity in dental resin composites to avoid unnecessary BPA exposure in patients.


Subject(s)
Benzhydryl Compounds , Composite Resins , Phenols , Phenols/analysis , Phenols/chemistry , Benzhydryl Compounds/chemistry , Composite Resins/chemistry , Materials Testing , Chromatography, High Pressure Liquid , Tandem Mass Spectrometry , Polyurethanes/chemistry , Polymethacrylic Acids/chemistry , Methacrylates/chemistry , Methacrylates/analysis , Polyethylene Glycols/chemistry , Polymerization
2.
J Prosthodont Res ; 2024 Apr 12.
Article in English | MEDLINE | ID: mdl-38616126

ABSTRACT

Purpose To assess elution from direct composite materials for provisional restorations and compare them with elution from direct restorative composites for permanent restorations.Methods Two dual-cure (Integrity Multi-Cure and Tempsmart DC) and two self-curing composites (Protemp 4 and Structur 3) were used, with Essentia serving as a reference. Cylindrical specimens (n=20) were cured according to the manufacturer's instructions; the dual-cure materials were prepared in both self- and dual-curing modes. Elution experiments were performed using water and absolute ethanol. The samples were incubated at 37 °C for either 24 h or four weeks; the extraction solvents were refreshed weekly. The eluted BisEMA (-3 / -6 / -10), BisGMA, CQ, UDMA, and TEGDMA were quantified using UHPLC-MS/MS.Results Monomer elution was detected in all provisional composites at 24 h and four weeks, but the amounts released did not exceed those released by the reference composite. When prepared in self-curing mode, Integrity Multi-Cure exhibited significantly higher elution of BisEMA-3, -6, and -10 in ethanol both after 24 h and cumulatively after four weeks. Self-cured Tempsmart DC released significantly more CQ, TEGDMA, and UDMA in both water and ethanol after immersion for 24 h and four weeks, along with significantly more BisGMA in ethanol both after 24 h and four weeks comparison to dual-cured Tempsmart DC (two-way ANOVA, post-hoc Tukey, P < 0.05).Conclusions Provisional composite materials did not elute higher amounts of monomers than a restorative composite. Dual-cured materials, prepared in the self-curing mode, show a trend towards higher monomer elution.

3.
Clin Oral Investig ; 27(12): 7189-7198, 2023 Dec.
Article in English | MEDLINE | ID: mdl-38051347

ABSTRACT

OBJECTIVES: Dental composites remain under scrutiny regarding their (long-term) safety. In spite of numerous studies on the release of monomers both in vitro and in vivo, only limited quantitative data exist on the in vivo leaching of degradation products from monomers and additives. The aim of this observational study was for the first time to quantitatively and qualitatively monitor the release of parent compounds and their degradation products in saliva from patients undergoing multiple restorations. MATERIALS AND METHODS: Five patients in need of multiple large composite restorations (minimally 5 up to 28 restorations) due to wear (attrition, abrasion, and erosion) were included in the study, and they received adhesive restorative treatment according to the standard procedures in the university clinic for Restorative Dentistry. Saliva was collected at different time points, starting before the restoration up until 24 h after the treatment with composite restorations. Saliva extracts were analyzed by liquid chromatography-mass spectrometry. RESULTS: Leaching of monomers and degradation products was highest within 30 min after the placement of the restorations. The highest median concentrations of monomers were recorded for UDMA, BisEMA-3, and TEGDMA; yet, besides BisEMA-3 and TEGDMA, no monomers could be detected after 24 h. Mono- and demethacrylated degradation products remained present up to 24 h and concentrations were generally higher than those of monomers. In patients with multiple restorations, degradation products were still present in the sample taken before the next operation, several weeks after the previous operation. CONCLUSIONS: Exposure to residual monomers and degradation products occurs in the first hours after restoration. Monomers are present in saliva shortly after restoration, but degradation products can be detected weeks after the restoration confirming a long-term release. CLINICAL SIGNIFICANCE: Future research should focus more on the release of degradation products from monomers and additives from resin-based materials given their prolonged presence in saliva after restoration.


Subject(s)
Composite Resins , Saliva , Humans , Composite Resins/chemistry , Saliva/chemistry , Polymethacrylic Acids/chemistry , Polyethylene Glycols/chemistry , Dental Materials/chemistry , Materials Testing , Dental Restoration, Permanent
4.
J Dent ; 116: 103894, 2022 01.
Article in English | MEDLINE | ID: mdl-34798152

ABSTRACT

OBJECTIVES: There is still much debate about the release of bisphenol A (BPA) from resin-based dental materials. Therefore, this study aimed to quantify BPA present as an impurity and to evaluate whether their degradation by salivary, bacterial, and chemical challenges could increase its release. METHODS: BPA was determined in three different amounts (300, 400, and 500 µg) of eight unpolymerized resin-based materials (four composites, one fissure sealant, two adhesives and one root canal sealer). Next, polymerized samples (n = 5) of each material were immersed in 1 mL of whole human pooled saliva collected from adults, Streptococcus mutans (2 × 107 CFU/mL), and acidic (0.1 M HCl), alkaline (0.1 M NaOH), and control media, respectively. The amount of BPA was quantified using an UPLC-MS/MS method including derivatization of BPA by pyridine-3-sulfonyl chloride. RESULTS: Only the composites contained trace amounts of BPA above the limit of quantification (ranging from 301±32 pg PBA/mg to 1534±62 pg BPA/mg), most likely as impurity from the synthesis of the monomers. The amounts of BPA released from polymerized materials upon salivary and bacterial degradation were too low for accurate quantification, but in water, quantifiable amounts of BPA were released from all materials. In alkaline media, the BPA release from two composites was significantly decreased, while the release from one adhesive was significantly increased, compared to water. CONCLUSIONS: BPA already present in unpolymerized resin-based materials may account for the release of BPA after polymerization. There was no clear indication that short-term material degradation leads to increased release of BPA.


Subject(s)
Composite Resins , Tandem Mass Spectrometry , Adult , Benzhydryl Compounds , Chromatography, Liquid , Dental Cements , Dental Materials , Humans , Phenols
5.
Dent Mater ; 38(1): 19-32, 2022 01.
Article in English | MEDLINE | ID: mdl-34774330

ABSTRACT

OBJECTIVES: Only little is known about degradation of methacrylate monomers. Therefore, using in vitro chemical and saliva degradation this study aimed to identify the degradation products of organic compounds present in resin-based dental materials. METHODS: Ten dental monomers and nine polymerized dental resin-based materials were immersed for 24 h in chemical media (0.1 M HCl, 0.1 M NaOH) and human pooled saliva in order to identify leached monomers and degradation products from chemical and saliva degradation. Samples were analyzed using liquid chromatography coupled to high-resolution mass spectrometry to identify previously unknown degradation products. RESULTS: During in vitro chemical degradation, uncured monomers were rapidly hydrolyzed into mono- and demethacrylated degradation products. During chemical degradation in alkaline conditions of polymerized materials, considered the worst-case scenario, only degradation products could be detected. In acidic conditions, monomers and their degradation products were detected. In addition, different additives such as EDMAB, DMPA and HMBP were present in acidic degradation samples. Degradation in human pooled saliva for 24 h to mimic the in vivo situation, resulted in the identification of both monomers and their degradation products. CLINICAL SIGNIFICANCE: Using state-of-the-art high-resolution mass spectrometry previously unknown degradation products of commonly used monomers were identified for the first time. Results show that patients may be exposed to monomers and their degradation products in the first 24 h after restorative procedures. The results provide a base for further research on the degradation of resin-based dental composites in order to assess their safety using elution and toxicity studies.


Subject(s)
Composite Resins , Dental Materials , Chromatography, Liquid , Composite Resins/chemistry , Dental Materials/chemistry , Humans , Materials Testing , Methacrylates , Saliva/chemistry
6.
Dent Mater ; 37(12): 1834-1844, 2021 12.
Article in English | MEDLINE | ID: mdl-34579959

ABSTRACT

OBJECTIVE: The biocompatibility of resin based dental composites has not yet been fully characterized even though certain monomers used in these composites are synthesized from Bisphenol A (BPA), a well-known estrogenic endocrine disruptor. As a result, they show structural relationship to BPA and can contain it as an impurity. Therefore, the estrogenic activity of 9 monomers, 2 photoinitiators, one photostabilizer and leachates of 4 commercially available composites was determined. METHODS: The ERα-CALUX bioassay was used to determine both agonistic and antagonistic estrogenic activities of the pure compounds (BPA, BisDMA, BisGMA, BisEMA(3), BisEMA(6), BisEMA(10), TEGDMA, TCD-DI-HEA, BADGE, UDMA, HMBP, DMPA, CQ) and the leachates of cured composite disks. The leachates of 4 commercially available composites (Solitaire 2, Ceram.x Spectra ST, G-ænial Posterior and Filtek Supreme XTE) in water and 0.1 M NaOH (pH = 13, 'worst-case scenario') were tested for estrogenic activity (pooled leachates from 10 cured composite disks). RESULTS: Agonistic estrogenic activity was found for the monomer BisDMA, the photostabilizer HMBP and photoinitiator DMPA. All leachates from the 4 tested composites showed significant agonistic estrogenic activity higher than the DMSO control, and the highest activity (potency and efficacy) was found for Solitaire 2, followed by Ceram.x Spectra ST. Furthermore, antagonistic estrogenic activity was found in the leachates from G-ænial Posterior. SIGNIFICANCE: These results show that significant estrogenic activity was found in all leachates of the cured composite disks, and that this estrogenicity is most likely due to a mixture effect of multiple estrogenic compounds (including BPA, HMBP and DMPA). This indicates that further research into the endocrine activity of all the compounds that are present in these composites (even at low quantities) and their possible mixture effect is warranted to guarantee their safe use.


Subject(s)
Dental Materials , Estrogen Receptor alpha , Biological Assay , Composite Resins , Materials Testing , Methacrylates
7.
Dent Mater ; 37(10): 1561-1568, 2021 10.
Article in English | MEDLINE | ID: mdl-34482962

ABSTRACT

OBJECTIVES: BPA release from composites on the short term has been reported in several in-vitro and in-vivo studies. However, it remains unclear whether these materials also leach BPA on the long term. Even though composites may release various (BPA-based) methacrylate monomers up to one year, quantitative data about BPA have not been reported due to the lack of a sensitive method to accurately quantify low levels of BPA. In this context, the aim of the study was to quantify the one-year release of BPA with an optimized analytical method. METHODS: Composite disks (n = 6, 6 mm diameter and 2 mm height) from four commercial materials (G-ӕnial Posterior, Venus, Ceram.x mono and Filtek Supreme XTE) were immersed in 1 mL of water or ethanol as extraction solvent and stored in the dark at 37 °C. The extraction solvent was renewed weekly for a period of 52 weeks. Samples were derivatized with pyridine-3-sulfonyl chloride before analysis with ultra-pressure liquid chromatography tandem mass spectrometry (UPLC-MS/MS). RESULTS: Derivatizing BPA increased the sensitivity of the analytical method and allowed accurate quantification of very low levels of BPA (i.e. 0.78 pmol BPA). BPA eluted continuously in ethanol from all four tested composites over a period of one year. BPA elution was clearly higher when ethanol was used as extraction solution. In water, BPA eluted could be detected up to one year, but levels could not be accurately quantified anymore after several weeks. SIGNIFICANCE: Composites can be considered as a potential long-term source of BPA, and thus should not be neglected when assessing the overall exposure to endocrine disrupting chemicals.


Subject(s)
Dental Materials , Tandem Mass Spectrometry , Benzhydryl Compounds/analysis , Chromatography, Liquid , Composite Resins , Materials Testing , Phenols
8.
Dent Mater ; 37(6): 1020-1029, 2021 06.
Article in English | MEDLINE | ID: mdl-33896600

ABSTRACT

OBJECTIVE: There is still much debate about the release of bisphenol-A (BPA) from dental materials. Therefore, this study aimed to quantify BPA present as an impurity in both BPA-based and non-BPA-based monomers and to evaluate whether these monomers may degrade to BPA upon salivary, bacterial, and chemical challenges. METHODS: BPA was determined in three different amounts (1, 2, and 3 µmol) of each monomer (TEGDMA, UDMA, mUDMA, BisGMA, BisEMA-3, -6, -10, -30, BisPMA, EBPADMA urethane, BADGE, and BisDMA). Next, the monomers (3 µmol) were immersed in whole human pooled saliva collected from adults, Streptococcus mutans (2 × 107 CFU/mL), and acidic (0.1 M HCl), alkaline (0.1 M NaOH), and control media. The amount of BPA was quantified using a specific and highly sensitive UPLC-MS/MS method including derivatization of BPA by pyridine-3-sulfonyl chloride. RESULTS: The monomers BisGMA and BisEMA-3 contained trace amounts (0.0006% and 0.0025%, respectively) of BPA as impurities of their synthesis process. BPA concentrations increased when the monomers BisGMA, BisEMA-3, BisEMA-6, BisEMA-10, BisPMA and BADGE were exposed to saliva and S. mutans, indicating degradation of a small amount of monomer into BPA. In addition, BisPMA and BADGE degraded into BPA under alkaline conditions. The conversion rate of the monomers into BPA ranged between 0.0003% and 0.0025%. SIGNIFICANCE: Impurities and degradation of BPA-based monomers may account for the release of BPA from resin-based dental materials. Even though the detected amounts of BPA due to monomer impurity were small, manufacturers of dental materials can reduce the BPA content by using only monomers of the highest purity. Considering the overall current trend towards BPA-free materials, it may be recommendable to investigate whether non-BPA based monomers can be used in dental resin-based materials.


Subject(s)
Composite Resins , Tandem Mass Spectrometry , Benzhydryl Compounds , Bisphenol A-Glycidyl Methacrylate , Chromatography, Liquid , Dental Materials , Humans , Materials Testing , Methacrylates , Phenols , Polyethylene Glycols , Polymethacrylic Acids
9.
Dent Mater ; 37(5): 894-904, 2021 05.
Article in English | MEDLINE | ID: mdl-33757655

ABSTRACT

OBJECTIVE: Incorporating silane-coupling agent into universal adhesives (UAs) to simplify adhesive luting of glass-ceramic restorations appeared ineffective due to silane's instability in an acidic aqueous solution. This study aimed to evaluate new silane technology added to an experimental UA to be bonded to glass ceramics without separate prior silanization. METHODS: Combined silane technology, consisting of 3-(aminopropyl)triethoxysilane (APTES) and γ-methacryloxypropyltriethoxysilane (γMPTES), was incorporated into an experimental UA formulation, being referred to as ADH-XTE (3M Oral Care). Immediate and aged shear bond strength (SBS) of ADH-XTE onto as-milled ('AM'), tribochemical silica-coated ('TSC'), HF-etched ('HF'), and mirror-polished ('MP') glass-ceramic CAD/CAM blocks (IPS e.max CAD) with/without separate silanization was measured (n = 10/group). The control adhesives included Scotchbond Universal ('SBU') and Scotchbond 1 XT ('SB1-XT'). The glass-ceramic surface topography and the fractography of the SBS-debonded specimens were observed by SEM. RESULTS: Without separate prior silanization, the experimental UA ADH-XTE, containing combined APTES/γMPTES silane technology, significantly outperformed the glass-ceramic bonding efficiency of its silane-containing SBU precursor, while it performed equally effective as SBU applied with prior silanization. Upon aging, significant reduction in SBS was recorded when ADH-XTE was bonded to TSC glass-ceramic surfaces (p < 0.05), while not to HF ones. Notably, the lowest SBS was obtained when the UAs were bonded to AM and MP glass-ceramic surfaces, in particular when applied without separate prior silanization (p < 0.05). SIGNIFICANCE: The glass-ceramic bonding capacity of the new combined APTES/γMPTES silane-containing UA ADH-XTE surpassed that of its SBU precursor. HF etching remains needed to durably bond to glass-ceramics.


Subject(s)
Dental Bonding , Silanes , Ceramics , Dental Cements , Dental Porcelain , Materials Testing , Resin Cements , Surface Properties , Technology
10.
Dent Mater ; 36(10): 1275-1281, 2020 10.
Article in English | MEDLINE | ID: mdl-32636078

ABSTRACT

OBJECTIVES: Indirect dental restorations produced by computer-aided design and computer-aided manufacturing (CAD/CAM) are relatively new in daily dental practice. The aim of the present study was to compare the monomer release between direct composite restorations and indirect CAD/CAM produced restorations (composite, ceramic and hybrid). METHODS: Identical crown restorations were prepared from three indirect materials (Cerasmart, Vitablocs Mark II and Vita Enamic) and one composite material (Clearfil AP-X). For each restoration, eight crown restorations were luted onto tooth samples and immersed into 2.5mL of an aqueous extraction solvent. Additionally, three nonluted crowns of each restoration type were also immersed in the extraction solvent, and served as controls. Every week, the extraction solvent was collected and refreshed, during a period of 8 weeks. The released monomers were quantified using ultra-performance liquid chromatography-tandem mass spectrometry. RESULTS: Indirect restorations release significantly lower quantities of residual monomers than direct restorations, and the monomers released by the luted indirect restorations are mainly derived from the composite material used for cementation. The quantity of monomers released by direct restorations greatly depended on the time of light polymerization. SIGNIFICANCE: In terms of monomer release, indirect restorations are a good alternative to direct restorations to limit patient exposure to residual monomers. It is important to ideally design the fit of indirect restoration so that the cement layer is as thin as possible and the monomer release from this cement layer remains as low as possible.


Subject(s)
Composite Resins , Dental Cements , Ceramics , Computer-Aided Design , Crowns , Dental Materials , Dental Porcelain , Dental Prosthesis Design , Humans , Materials Testing
11.
Toxicol Lett ; 332: 7-13, 2020 Oct 10.
Article in English | MEDLINE | ID: mdl-32615244

ABSTRACT

Root canal sealers are commonly used to endodontically treat teeth with periapical infections. Some root canal sealers based on epoxy resin contain bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE). The presence of these chemicals is of concern due to the close contact to the blood stream at the apex and the long setting times of up to 24 h. These chemicals, or any of their degradation products or metabolites, can then exert their toxic effects before being excreted. This study aimed to identify the phase I in vitro biotransformation products of BADGE and BFDGE using human liver microsomes. During incubation with microsomal fractions, the epoxides were rapidly hydrolysed in a NADPH independent manner resulting in the formation of BADGE.2H2O and BFDGE.2H2O. Further, oxidative reactions, such as hydroxylation and carboxylation, generated other BADGE metabolites, such as BADGE.2H2O-OH and BADGE.H2O.COOH, respectively. For BFDGE, further oxidation of BFDGE.2H2O led to the newly reported carboxylic acid, BFDGE.H2O.COOH. In total, three specific metabolites have been identified which can serve in future human biomonitoring studies of BADGE and BFDGE.


Subject(s)
Benzhydryl Compounds/pharmacokinetics , Epoxy Compounds/pharmacokinetics , Liver/metabolism , Root Canal Filling Materials/pharmacokinetics , Benzhydryl Compounds/toxicity , Biotransformation , Carboxylic Acids/metabolism , Epoxy Compounds/toxicity , Female , Humans , Hydroxylation , Male , Microsomes, Liver/metabolism , NADP/metabolism , Oxidation-Reduction , Root Canal Filling Materials/toxicity
12.
ACS Appl Mater Interfaces ; 12(27): 30120-30135, 2020 Jul 08.
Article in English | MEDLINE | ID: mdl-32530270

ABSTRACT

Apart from producing high bond strength to tooth enamel and dentin, a dental adhesive with biotherapeutic potential is clinically desirable, aiming to further improve tooth restoration longevity. In this laboratory study, an experimental two-step universal adhesive, referred to as Exp_2UA, applicable in both the etch-and-rinse (E&R) and self-etch (SE) modes and combining a primer, containing 10-methacryloyloxydecyldihydrogen phosphate as a functional monomer with chemical binding potential to hydroxyapatite, with a bioglass-containing hydrophobic adhesive resin, was multifactorially investigated. In addition to primary property assessment, including measurement of bond strength, water sorption, solubility, and polymerization efficiency, the resultant adhesive-dentin interface was characterized by transmission electron microscopy (TEM), the filler composition was analyzed by energy-dispersive X-ray spectroscopy, and the bioactive potential of the adhesive was estimated by measuring the long-term ion release and assessing its antienzymatic and antibacterial potential. Four representative commercial adhesives were used as reference/controls. Application in both the E&R and SE modes resulted in a durable bonding performance to dentin, as evidenced by favorable 1 year aged bond strength data and a tight interfacial ultrastructure that, as examined by TEM, remained ultramorphologically unaltered upon 1 year of water storage aging. TEM revealed a 20 µm thick hydrophobic adhesive layer with a homogeneous bioglass filler distribution. Adequate polymerization conversion resulted in extremely low water sorption and solubility. In situ zymography revealed reduced endogenous proteolytic activity, while Streptococcus mutans biofilm formation was inhibited. In conclusion, the three-/two-step E&R/SE Exp_2UA combines the high bonding potential and bond degradation resistance with long-term ion release, rendering the adhesive antienzymatic and antibacterial potential.


Subject(s)
Anti-Bacterial Agents/chemistry , Calcium/chemistry , Fluorides/chemistry , Zinc Compounds/chemistry , Anti-Bacterial Agents/pharmacology , Biofilms/drug effects , Dentin-Bonding Agents , Materials Testing , Microscopy, Electron, Transmission , Resin Cements/chemistry , Streptococcus mutans/drug effects , Tensile Strength
13.
Eur J Oral Sci ; 128(3): 233-240, 2020 06.
Article in English | MEDLINE | ID: mdl-32378254

ABSTRACT

The aim of this study was to investigate the protection efficiency of two types of face masks against composite dust and to characterize the particles that penetrated through the masks. Composite dust was created by grinding a commercial nano-filled composite in a plexiglass box without using water cooling or high vacuum evacuation, in order to obtain a worst-case exposure. Dust particles were collected using a personal inhalable aerosol sampler (IOM) fixed inside a custom-made phantom head. Surgical and filtering facepiece (FFP3) masks were tested, and the situation without a mask served as control. The IOM sampler contained a cassette with two filters to collect large inhalable (4-100 µm) and respirable dust particles (<4 µm). The amount of particles was determined gravimetrically by weighing filters before and after composite grinding, and further characterized by electron microscopy. Particle collection for both inhalable and respirable dust was the highest when no mask was used, and the lowest with the use of a FFP3 mask. Different sizes and shapes of particles were observed, with the largest particles (>1 µm) being seen when no mask was applied, whereas only nanoparticles could be detected when either type of face mask was applied. Even though FFP3 masks showed a higher filtration efficacy than surgical masks of the inhalable dust fraction, penetration of a small respirable particle fraction was inevitable for both masks.


Subject(s)
Dust , Occupational Exposure , Aerosols , Filtration , Masks , Occupational Exposure/analysis , Particle Size
14.
Part Fibre Toxicol ; 17(1): 10, 2020 02 26.
Article in English | MEDLINE | ID: mdl-32101144

ABSTRACT

BACKGROUND: The terms agglomerates and aggregates are frequently used in the regulatory definition(s) of nanomaterials (NMs) and hence attract attention in view of their potential influence on health effects. However, the influence of nanoparticle (NP) agglomeration and aggregation on toxicity is poorly understood although it is strongly believed that smaller the size of the NPs greater the toxicity. A toxicologically relevant definition of NMs is therefore not yet available, which affects not only the risk assessment process but also hinders the regulation of nano-products. In this study, we assessed the influence of NP agglomeration on their toxicity/biological responses in vitro and in vivo. RESULTS: We tested two TiO2 NPs with different primary sizes (17 and 117 nm) and prepared ad-hoc suspensions composed of small or large agglomerates with similar dispersion medium composition. For in vitro testing, human bronchial epithelial (HBE), colon epithelial (Caco2) and monocytic (THP-1) cell lines were exposed to these suspensions for 24 h and endpoints such as cytotoxicity, total glutathione, epithelial barrier integrity, inflammatory mediators and DNA damage were measured. Large agglomerates of 17 nm TiO2 induced stronger responses than small agglomerates for glutathione depletion, IL-8 and IL-1ß increase, and DNA damage in THP-1, while no effect of agglomeration was observed with 117 nm TiO2. In vivo, C57BL/6JRj mice were exposed via oropharyngeal aspiration or oral gavage to TiO2 suspensions and, after 3 days, biological parameters including cytotoxicity, inflammatory cell recruitment, DNA damage and biopersistence were measured. Mainly, we observed that large agglomerates of 117 nm TiO2 induced higher pulmonary responses in aspirated mice and blood DNA damage in gavaged mice compared to small agglomerates. CONCLUSION: Agglomeration of TiO2 NPs influences their toxicity/biological responses and, large agglomerates do not appear less active than small agglomerates. This study provides a deeper insight on the toxicological relevance of NP agglomerates and contributes to the establishment of a toxicologically relevant definition for NMs.


Subject(s)
DNA Damage , Epithelial Cells/drug effects , Nanoparticles/toxicity , Titanium/toxicity , Administration, Oral , Animals , Bronchoalveolar Lavage Fluid/chemistry , Caco-2 Cells , Cell Survival/drug effects , Female , Humans , Inhalation Exposure/adverse effects , Mice, Inbred C57BL , Nanoparticles/chemistry , Particle Size , Surface Properties , THP-1 Cells , Titanium/chemistry
15.
J Adhes Dent ; 22(1): 65-77, 2020.
Article in English | MEDLINE | ID: mdl-32030377

ABSTRACT

PURPOSE: This study investigated the bonding efficacy of a new so-called self-adhesive composite hybrid onto flat (FLAT) and high C-factor class-I cavity-bottom (CAVITY) dentin. MATERIALS AND METHODS: The immediate and aged (50,000 thermocycles) microtensile bond strength (µTBS) to FLAT and CAVITY dentin of the experimental self-adhesive bulk-fill restorative (K-0180 ASAR pilot [ASAR-pilot], Dentsply Sirona) was compared to that of two universal adhesives applied in self-etch mode and combined with a bulk-fill composite (Prime&Bond Elect/QuiXfil [P&Be/QuiXF], Prime&Bond Active/QuiXfil [P&Ba/QuiXF], both Dentsply Sirona), two pre-conditioned materials (Activa Bioactive-Restorative [Activa], Pulpdent; Fuji II LC Improved [Fuji2LC], GC); and one bulk-fill glass-hybrid restorative (Equia Forte Fil [EquiaF], GC). Statistically significant differences were recorded using Welch's ANOVA with Games-Howell contrast (p < 0.05). RESULTS: No significant difference in immediate µTBS was recorded when the restorative materials were applied onto FLAT dentin, except for Activa_FLAT and EquiaF_FLAT. When bonded to CAVITY dentin, the significantly highest µTBS was recorded for Fuji2LC_CAVITY (layer filled), and was not significantly different only from P&Ba/QuiXF_CAVITY. Upon aging, the highest µTBS to flat dentin was achieved by ASAR-pilot_FLAT, which was not significantly different from P&Be/QuiXF_FLAT and Fuji2LC_FLAT. No significant difference between immediate and aged µTBS was recorded for ASAR-pilot when bonded onto FLAT or CAVITY dentin; the latter, however, was associated with low bond strength. CONCLUSION: Favorable bonding performance was found for the new self-adhesive bulk-fill composite hybrid ASAR-pilot when bonded to flat dentin. However, much lower bond strength was recorded when ASAR-pilot was bonded to high C-factor cavity-bottom dentin.


Subject(s)
Dental Bonding , Dentin-Bonding Agents , Composite Resins , Dental Cements , Dentin , Materials Testing , Resin Cements , Tensile Strength
16.
J Adhes Dent ; 22(1): 85-97, 2020.
Article in English | MEDLINE | ID: mdl-32030379

ABSTRACT

PURPOSE: The material structure and chemical elemental composition of a new self-adhesive composite hybrid were investigated. The bonding performance when applied on flat (FLAT) vs high C-factor class-I cavity-bottom (CAVITY) dentin and in light-cure (LC) vs self-cure (SC) mode was determined. MATERIALS AND METHODS: The self-adhesive bulk-fill composite Surefil One (Su-O; Dentsply Sirona) was compared with the resin-modified glass-ionomer Fuji II LC Improved (Fuji2LC; GC) and the ion-releasing alkasite material Cention N (CentionN; Ivoclar Vivadent). The material structure was examined with SEM and TEM, while the chemical elemental composition was analyzed using EDS. The immediate and aged microtensile bond strength (µTBS) of Su-O_LC/SC was compared to that of Fuji2LC applied without any pre-treatment, and to that of CentionN applied following bonding with Adhese Universal (AU) (Ivoclar Vivadent) in self-etch mode (AU/CentionN). All restorative materials were bonded onto FLAT and CAVITY dentin. Statistical analysis was performed with the Kruskal-Wallis nonparametric test. RESULTS: EDS analysis revealed that Su-O was richer in C and P than the reference restorative materials. Applied to FLAT dentin, the significantly highest immediate and aged µTBS were recorded for AU/CentionN, which were not significantly different only from Su-O_LC. Applied to CAVITY dentin, the significantly highest immediate µTBS was recorded for AU/CentionN, which did not differ significantly only from Su-O_SC. Su-O_LC bonded to CAVITY dentin suffered from a high incidence of pre-test failures. CONCLUSION: While Su-O_LC bonded effectively and durably to FLAT dentin, Su-O_SC bonded more favorably than Su-O_LC in class-I cavities, which was probably related to shrinkage stress variously challenging the respective bond.


Subject(s)
Dental Bonding , Dentin-Bonding Agents , Composite Resins , Dental Cements , Dentin , Materials Testing , Resin Cements , Tensile Strength
17.
Clin Oral Investig ; 24(2): 683-691, 2020 Feb.
Article in English | MEDLINE | ID: mdl-31123872

ABSTRACT

OBJECTIVES: The objectives of this cross-sectional survey were to determine the prevalence of secondary caries (SC) in general population, to identify patient- and material-related factors which may affect the prevalence, and to describe some clinical characteristics of SC lesions. MATERIALS AND METHODS: A total of 4036 restorations in 450 patients, who visited the university dental clinic for a regular (half) yearly checkup, were examined clinically (and radiographically) for the presence of SC. Clinical characteristics of the detected SC lesions (size, activity, and location) and the planned treatment were recorded. In addition, patients' caries-risk status was assessed according to the modified "cariogram" model. RESULTS: In total, 146 restorations were diagnosed with SC, which gives an overall prevalence of 3.6%. Restorative material, restoration class, patient's caries risk, and smoking habits were shown to be important factors, as SC prevalence was significantly higher with composites, class II restorations, high-caries-risk patients, and smokers. Restorations' gingival margins were most frequently affected by SC. The largest number of restorations with SC (72%) was scheduled for the replacement. CONCLUSIONS: Prevalence of SC was higher with composite than with amalgam restorations, irrespective of the patient's caries-risk status. Gingival margins of class II, including MOD restorations, seem to be the place of less resistance to SC development. Management of SC seems to place a considerable burden on the health care workforce and expenditure. CLINICAL RELEVANCE: Secondary caries (SC) is considered to be the main cause of dental restoration failure and one of the biggest clinical challenges related to dental composites. Nevertheless, its prevalence in daily practice is still not clear, which impedes an accurate estimation of its impact on health care costs.


Subject(s)
Dental Caries , Composite Resins , Cross-Sectional Studies , Dental Amalgam , Dental Restoration Failure , Dental Restoration, Permanent , Humans , Prevalence
18.
Clin Oral Investig ; 24(7): 2403-2414, 2020 Jul.
Article in English | MEDLINE | ID: mdl-31811493

ABSTRACT

OBJECTIVE: To evaluate the collection efficiency of water spray on the release of airborne composite particles during grinding of composite materials. MATERIALS AND METHODS: Composite sticks (L:35 mm × W:5.4 mm × H:1.6 mm) of seven commercial dental composites were ground with a rough diamond bur (grain size 100 µm, speed 200,000 rpm). All experiments were performed in an enclosed 1-m3 chamber with low particulate background (< 1,000 #/cm3), and airborne particles were evaluated based on their electrical mobility. The number size distribution was determined by scanning mobility particle sizer (SMPS). Particles were collected by an electrostatic precipitator (ESP), and were ultramorphologically and chemically analyzed by a transmission electron microscope equipped with energy-dispersive X-ray spectroscopy (TEM-EDS). RESULTS: SMPS measurements confirmed that both dry and wet grinding generated high concentrations of nanoparticles particles with the highest concentration recorded during the last minute of grinding (1.80 × 106 - 3.29 × 106#/cm3), after which a gradual decline in particle concentration took place. Nevertheless, grinding with water spray resulted in a significant reduction of the number of released particles (5.6 × 105 - 1.37 × 106#/cm3). The smallest particle diameter was recorded during the last minute of grinding followed by a continuous growth for every next measurement. TEM of composite dust revealed a high concentration of particles varying in both size and shape. CONCLUSIONS: Regardless of whether the water cooling spray system was used during bur manipulation of composite materials, predominately nanoparticles were released. However, the particle concentrations were significantly decreased with water spray. CLINICAL RELEVANCE: Since water spray might not be sufficient in nanoparticle collection, special care should be taken to prevent inhalation of composite dust.


Subject(s)
Dust , Nanoparticles , Particle Size , Water
19.
Dent Mater ; 36(2): 270-283, 2020 02.
Article in English | MEDLINE | ID: mdl-31852585

ABSTRACT

OBJECTIVE: To determine the cytotoxic and genotoxic potential of the respirable fraction of composite dust (<4 µm) on human bronchial epithelial cells. METHODS: Composite sticks of three commercial dental composites (Filtek Supreme XTE, Grandio, Transbond XT) were ground in an enclosed plexiglass chamber with a rough dental bur (grain-size 100 µm) and the generated airborne respirable dust was collected in a personal cyclone on a teflon filter (pore size 5 µm). Immediately after particle collection, the dust was quantified gravimetrically and the particles were suspended in cell culturing medium. Next, human bronchial epithelial cells (16HBE14o-) were exposed to the suspensions (3 µg/ml-400 µg/ml). After 24 h, cell viability (WST-1 assay) and membrane integrity (LDH assay) were evaluated. Furthermore, the genotoxic effect of a sub-cytotoxic concentration (50 µg/ml) of composite dust was evaluated by the comet assay after 3 h exposure and cell cycle disturbances were analyzed by flow cytometry. Cellular uptake of particles was evaluated by transmission electronic microscope (TEM). RESULTS: For all three tested composite materials, a decrease in metabolic activity of 10-35% was observed when the cells were exposed to the highest concentrations (100 µg/ml-400 µg/ml). Toxicity was partially linked to membrane disruption especially after 72 h exposure. All tested composites provoked a mild genotoxic effect after short-term exposure compared to the control groups. TEM revealed that respirable particles of all tested composites were taken up by the cells. SIGNIFICANCE: The respirable fraction of composite dust only showed cytotoxic effects at the highest concentrations, whereas mild genotoxicity was observed after exposure to a sub-cytotoxic concentration.


Subject(s)
Dust , Occupational Exposure , Comet Assay , DNA Damage , Dental High-Speed Equipment , Humans , Particle Size
20.
Dent Mater ; 35(10): 1415-1429, 2019 10.
Article in English | MEDLINE | ID: mdl-31421958

ABSTRACT

OBJECTIVE: Enamel bond durability of three new alternative etchants combined with three representative adhesives was determined. METHODS: The 'immediate' and 'aged' micro-tensile bond strength (µTBS) of the 3-step etch&rinse adhesive OptiBond FL ('O-FL', Kerr), 2-step self-etch (SE) adhesive Clearfil SE Bond 2 ('C-SE2', Kuraray Noritake) and universal adhesive Adhese Universal ('ADU', Ivoclar Vivadent) were measured when bonded to enamel following either a proprietary organic acid-containing Enamel Conditioner ('EC', Shofu), a phosphoric-acid monomer-containing Multi Etchant ('ME', Yamakin: 10-methacryloyloxy tetraethylene glycol dihydrogenphosphate or MTEGP), or a metal salt-based ZON etchant ('ZON', Ivoclar Vivadent: ZrO(NO3)2). All alternative etchants were used in replacement of phosphoric acid, the latter (K-Etchant, Kuraray Noritake) also used with O-FL and ADU, in addition to C-SE2 that was solely used in SE mode (controls). The enamel-etching patterns and de-bonded fracture surfaces were examined by SEM, while the interfaces with enamel were ultra-morphologically characterized by TEM. RESULTS: No statistically significant difference in immediate and aged µTBS, obtained by combining the three alternative etchants with the three adhesives, was recorded as compared with the respective controls, except for ME combined with O-FL. Upon aging, significant reduction in µTBS was recorded for the ME/C-SE2 and ME/ADU combinations. The percentage of adhesive failures increased with aging. SEM revealed similar etching patterns produced by EC and ZON as by classic phosphoric-acid etching, for which also numerous micro-resin tags at the adhesive-enamel interface were disclosed. SIGNIFICANCE: Durable bonding to enamel was generally obtained for all etchant/adhesive combinations with the exception of the ME/O-FL combination.


Subject(s)
Dental Bonding , Dentin-Bonding Agents , Acid Etching, Dental , Dental Cements , Dental Enamel , Dentin , Materials Testing , Resin Cements , Tensile Strength
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