Modification of a universal adhesive with CHX- or DOX-loaded TiO2 nanotubes as an anti-MMP strategy.

This article presents details of fabrication, biological activity (i.e., anti–matrix metalloproteinase [anti-MMP] inhibition), cytocompatibility, and bonding characteristics to dentin of a unique doxycycline (DOX)–encapsulated halloysite nanotube (HNT)–modified adhesive. We tested the hypothesis that the release of DOX from the DOX-encapsulated nanotube-modified adhesive can effectively inhibit MMP activity. We incorporated nanotubes, encapsulated or not with DOX, into the adhesive resin of a commercially available bonding system (Scotchbond Multi-Purpose [SBMP]). The following groups were tested: unmodified SBMP (control), SBMP with nanotubes (HNT), and DOX-encapsulated nanotube-modified adhesive (HNT+DOX). Changes in degree of conversion (DC) and microtensile bond strength were evaluated. Cytotoxicity was examined on human dental pulp stem cells (hDPSCs). To prove the successful encapsulation of DOX within the adhesives—but, more important, to support the hypothesis that the HNT+DOX adhesive would release DOX at subantimicrobial levels—we tested the antimicrobial activity of synthesized adhesives and the DOX-containing eluates against Streptococcus mutans through agar diffusion assays. Anti-MMP properties were assessed via β-casein cleavage assays. Increasing curing times (10, 20, 40 sec) led to increased DC values. There were no statistically significant differences (p > .05) in DC within each increasing curing time between the modified adhesives compared to SBMP. No statistically significant differences in microtensile bond strength were noted. None of the adhesives eluates were cytotoxic to the human dental pulp stem cells. A significant growth inhibition of S. mutans by direct contact illustrates successful encapsulation of DOX into the experimental adhesive. More important, DOX-containing eluates promoted inhibition of MMP-1 activity when compared to the control. Collectively, our findings provide a solid background for further testing of encapsulated MMP inhibitors into the synthesis of therapeutic adhesives that may enhance the longevity of hybrid layers and the overall clinical performance of adhesively bonded resin composite restorations.

To assess the resin microtensile bond strength (MTBS) and the degree of conversion (DC) of indirect composite resin restorations polymerized with light and heat. Two direct (Filtek Z100 and Premise) and one indirect (Premise Indirect) composite resins were polymerized with a combination of light and heat (138°C for 20 min). For MTBS, 42 cylinders were fabricated (n = 7). After the surface treatment, cylinders were bonded to each other using adhesive resin (Optibond FL). Specimens were stored in water for 24 h. Another 15 cylinders (n = 5) were fabricated for determining degree of conversion using Fourier Transform Infrared Spectrometry immediately and at 24 h. The MTBS and the DC was submitted to two-way ANOVA. The interaction with existing data was explored with univariate ANOVA and two-way ANOVA. Tukey's HSD post-hoc test was used to detect pairwise differences (α = 0.05). The MTBS to light and heat polymerized Z100 was 75.7 MPa, significantly higher than that to Premise (58.6 MPa) and Premise Indirect (63.9 MPa). The immediate DC for Z100, Premise, and Premise Indirect were 51.0%, 68.7%, and 61.8%, respectively. The DC at 24 h ranged from 53.4% (Z100) to 72.8% (Premise Indirect) and significantly increased for Premise Indirect only. Comparison with previously published data revealed that the heat treatment increased both MTBS and DC of Premise and Premise Indirect. Z100 showed better bond strength but lower DC. Heat treatment and a 24-h delay before delivery can benefit DC of Premise Indirect. The increase in DC of Premise and Premise Indirect did not affect their bond strength.

To evaluate the influence of heat application on the degree of conversion (DC) of the 3M Single Bond Universal Adhesive System, as well as its transdentinal cytotoxicity and microtensile bond strength to dentin. Experimental groups were established according to the time and temperature of the air jet: G1: 5 seconds-25°C; G2: 10 seconds-25°C; G3: 20 seconds-25°C; G4: 5 seconds-50°C; G5: 10 seconds-50°C; G6: 20 seconds-50°C. In control group (G7), no treatment was performed. The DC was assessed using the Fourier transform infrared spectroscopy-attenuated total reflectance (FTIR-ATR) technique. For the transdentinal cytotoxicity test, dentin discs fitted in artificial pulp chambers (APC) received the application of the adhesive system and the air jets. For the microtensile bond strength, healthy molars were restored and submitted to the microtensile test after 24 hours and 6 months, respectively. Significant reduction in viability of Mouse Dental Papilla Cell-23 (MDPC-23), which exhibited morphological changes, was observed in all experimental groups compared to control (p<0.05). Although all tested protocols resulted in transdentinal diffusion of 2-hydroxyethyl methacrylate (HEMA), the group G6 presented the highest degree of monomeric conversion and the lowest cytotoxic effect, with higher dentin bond strength values in comparison to group G1 (p<0.05). Applying an air blast at 50°C for 20 seconds increases the DC and microtensile bond strength of the 3M Single Bond Universal Adhesive System to dentin, as well as reduces the transdentinal cytotoxicity of the material to pulp cells.

To assess micro-tensile bond strength (μTBS), degree of conversion (DC), microleakage (ML) antibacterial efficacy, and adhesive remnant index (ARI) of orthodontic brackets to enamel with different concentrations of photoactivated riboflavin-doped hydroxyapatite (HA) nanospheres (NS) (0%,1%,5% and 10%) and 0.5 wt% RF alone in orthodontic adhesive. Samples were included on the predefined inclusion criteria and positioned up to the cementoenamel junction (CEJ). Hydroxy apatite nanospheres (HANS) commercially bought were doped with RF. Surface characterization of HANS and RF-doped HANS were assessed along with EDX analysis. Samples were grouped based on experimental orthodontic adhesive modification. Group 1: Transbond XT no modification, Group 2: experimental Transbond XT 0.5 wt% RF, Group 3: experimental Transbond XT 0.5 wt% RF-doped 1% HANS, Group 4: experimental Transbond XT 0.5 wt % RF-doped 5% HANS and Group 5: Experimental Transbond XT 0.5 wt% RF-doped 10% HANS. Brackets were placed based on different adhesive modifications and samples underwent thermocycling. Samples were evaluated for μTBS, DC, and ML. The type of failure was assessed using ARI. Adhesive modified and un-modified in four different concentrations (0%, 1%, 5%, and 10%) and 0.5 wt% RF only were used to test efficacy against Streptococcus mutans (S.mutans). The survival rate of S.mutans and ML was determined using the Kruskal-Wallis Test. For the analysis of μTBS, ANOVA was employed, followed by a post-hoc Tukey HSD multiple comparisons test. The highest μTBS and lowest ML were observed in Group 2 experimental Transbond XT 0.5 wt% RF only. The lowest μTBS, highest ML, and lowest DC was seen in Group 5 experimental Transbond XT 0.5 wt% RF-doped 10% HANS. Samples in Group 1 in which Transbond XT was used as adhesive demonstrated significantly the highest microbial count of S.mutans and DC. Photoactivated RF-doped HANS in 1% and 0.5 wt% Riboflavin alone in orthodontic adhesive for metallic bracket bonding improved micro tensile bond strength, ML, DC, and antibacterial scores. RESEARCH HIGHLIGHTS: The highest μTBS and lowest ML were observed in Group 2 experimental Transbond XT 0.5 wt% RF only. The lowest μTBS, highest ML, and lowest DC was seen in Group 5 experimental Transbond XT 0.5 wt% RF-doped 10% HA-NS. Samples in Group 1 in which Transbond XT was used as adhesive demonstrated significantly the highest microbial count of S.mutans and DC.

Influence of ceramic veneer on the transdentinal cytotoxicity, degree of conversion and bond strength of light-cured resin cements to dentin

This study investigated the effects of adding tricalcium silicate nanoparticles (TCSNp) to the universal G2 bond adhesive (G2BU) in self-etch (SE) mode on shear bond strength (SBS) to orthodontic brackets, cytotoxicity, and degree of conversion (DC). A total of 176 human teeth were divided into four groups based on TCSNp concentration in G2BU adhesive: 0% (control), 1%, 3%, and 5%. The G2BU adhesive consists of a hydrophilic primer (P) and a hydrophobic bonding agent (2B). TCSNp were added to the 2B component by mixing 0.1, 0.3, and 0.5 g of TCSNp with 9.9, 9.7, and 9.5 g of 2B, respectively. SBS was assessed after 24 h of water storage and 5000 thermocycles using a universal testing machine. Cytotoxicity was evaluated using the MTT assay on rat embryo fibroblast cells, and DC was measured using fourier-transform infrared spectroscopy. Statistical analysis included one-way ANOVA and Tukey's post-hoc test, with significance set at p < 0.05. After 24 h, mean SBS values were 15.58 MPa (control), 13.66 MPa (1% TCSNp), 15.99 MPa (3% TCSNp), and 12.04 MPa (5% TCSNp). After 5000 thermocycles, SBS values decreased to 12.91 MPa (control), 12.42 MPa (1% TCSNp), 11.11 MPa (3% TCSNp), and 10.21 MPa (5% TCSNp). ANOVA showed significant differences between groups (p < 0.05), except between the control and 3% TCSNp groups. Cell viability increased with higher TCSNp concentrations, with significant differences at 72 h between control and 5% TCSNp groups (p = 0.014). Mean DC values were 51.66% (control), 49.33% (1% TCSNp), 49.66% (3% TCSNp), and 48% (5% TCSNp). ANOVA indicated no significant differences between groups. Adding TCSNp to G2BU in SE mode maintains clinically acceptable SBS levels and enhances cytocompatibility. Higher TCSNp concentrations may reduce SBS and DC slightly. Further studies are needed to evaluate long-term effects.

Impact of drug loading on release from levonorgestrel intrauterine systems

Background: The problem of composite resin filling is the longer time consumed for incremental application. Bulk-fill composite resins were introduced to the market as substitutes for dental amalgam for restoration of posterior teeth. Objectives: The aim of this study was to evaluate the curing depth and degree of conversion of two bulk-fill composite resins. Materials and methods: . Specimens of specific dimensions were prepared from Glacier and SureFil (universal shade, A2), they classified as bulk-fill composite resins. Depth of cure, degree of conversion at different thicknesses for each material (2,3,4,5 and 6 mm) for each thickness separately. The curing depth was determined by the scrapping method (ISO 4049, 2000). The degree of conversion was measured by the Buker FTIR Spectroscopy. Results: The results indicated that, Glacier composite resin has greater curing depth than that of SureFil composite resin. Glacier composite resin was cured above 6 mm thickness, while SureFil composite resin was cured above 5 mm. In general, the degree of conversion was different at the different thicknesses of the materials. SureFil composite resin showed highest degree of conversion at 3 mm followed by 2 mm thickness, while the lowest degree of conversion was noted at 6 mm thickness. Glacier composite resin has the highest degree of conversion at 3 mm followed by 2 mm thickness, while the lowest degree of conversion was noted at 6 mm thickness. SureFil showed positive correlation between the depth of cure and the degree of conversion. Glacier composite resin showed no significant correlation between the depth of cure and degree of conversion. Conclusions: The studied bulk-fill composite resins, cured up to 5mm to 6mm thicknesses. 2 and 3mm thicknesses adequately polymerized than 4 mm, 5 mm and 6 mm thicknesses. The degree of conversion of 2 mm and 3 mm thicknesses was greater than that of the other thicknesses. There was positive correlation between the degree of conversion and curing depth of SureFil composite resin. On the other hand, Glacier composite resin showed no significant correlation between the depth of cure and degree of conversion.

Adhesive performance of a multi-mode adhesive system: 1-Year in vitro study

Objective To assess the effect of 10% doxycycline (DOX) compared to 2% chlorhexidine (CHX) on the longevity of dentin-bond strength. Methods Sixty-six extracted molars were collected and prepared and divided into two groups based on the test to be performed. Group I (n=48) for the micro-tensile bond strength (µTBS) test and Group II (n=18) for the confocal laser scanning microscopy (CLSM) test. Group I was divided into 3 subgroups (n=16) according to pretreatment agent following acid etching. Group A (control): without pretreatment, group B: 10% Doxycycline pretreatment, Group C: 2% Chlorhexidine pretreatment. Palfique universal bond (PU) and Composite resin were applied according to the manufacturer's instructions. Group II was divided into 3 subgroups (n=6) based on the same pretreatment protocols used in Group I. However, for resin-dentin bond evaluation using CLSM, 0.1 mg/mL Rhodamine B fluorescent dye was mixed with the adhesive. After that, all subgroups of group I and group II were subdivided into 2 subdivisions:(T1) without thermocycling and (T2) thermocycling for 10000 cycles. µTBS testing was achieved via a digital universal testing machine. The failure mode was tested by a stereomicroscope (30x magnification). Results Intergroup comparison of mean µTBS values (MPa) was performed using one-way ANOVA, then by Tukey post-hoc test with statistical significance at p ≤ 0.016. In contrast, intragroup comparison was achieved using a paired t-test with a statistical significance of p ≤ 0.05. Comparison between categorical data was made using a chi-square test. The 10% DOX pretreatment group showed significantly higher µTBS values than CHX and the control group with and without thermocycling (p &lt; 0.001). No statistically significant difference in failure modes was recorded among groups without and with thermocycling. There was no correlation between µTBS and failure mode performed using Spearman’s rank correlation. CLSM revealed that the 10% DOX group exhibited greater resin infiltration with a thicker hybrid layer. Both matrix metalloproteinase (MMP) inhibitors created a uniform hybrid layer. Conclusions Pre-treatment with MMP inhibitors might have inhibited the degradation of resin-dentin interfaces. In addition, 10% DOX pretreatment for 60 seconds after etching appears to be more efficient in enhancing the durability of the bond. Additionally, the composition of PU may influence bond strength, warranting further investigation. Moreover, thermocycling may adversely impact the micro-tensile bond strength.

Objective: The objective was to evaluate the influencing factors in the fabrication of gelatin matrix (gelatin chips) for drug delivery. The attributes affecting drug release characteristics of the gelatin products were examined.Significance: Understanding the attributes that affect drug release from gelatin matrix could provide the knowledge base for the development, manufacturing, and performance evaluation of gelatin-based drug products for sustained drug delivery.Methods: Chlorhexidine (CHX) was the model drug in the gelatin-product testing. The gelatin products were fabricated by two methods: a single-pot mixing of all the components and a two-step gelatin crosslinking followed by drug loading. Different gelatin types (Type A porcine and Type B bovine), glutaraldehyde (GTA) crosslinking conditions, glycerin concentration, and CHX concentration in drug loading and loading time were used to fabricate the products. The cumulative amounts of CHX release from the gelatin products were determined using in vitro release testing (IVRT).Results: The attributes affecting CHX release from the gelatin products were gelatin type, GTA crosslinking, and CHX loading concentration. The fabrication methods (two-step method of gelatin crosslinking and drug loading by equilibration vs. direct mixing of the components) also affected CHX release. Other attributes such as glycerin and CHX loading time did not show significant effects on drug release under the conditions studied. In addition, the results in the two IVRT methods employed in this study were comparable.Conclusion: Gelatin products of qualitative (Q1) and quantitative (Q2) differences could lead to different drug release behaviors. Drug release was also affected by the ingredient mixing steps during gelatin chip fabrication.

This study assessed the effect of antioxidants vitamin C (Vit. C), vitamin E (Vit. E) and quercetin (Querc) on the dentin bonding performance, degree of conversion, and rate of polymerization of three commercial adhesive systems (Adper Single Bond 2 [SB], Clearfil SE Bond [CSE], Adper Easy Bond [EB]). Human premolars were restored using antioxidant-doped adhesives. The samples were stored for 24 h in distilled water or 6 months under simulated pulpal pressure. Teeth were cut into sticks and the microtensile bond strength (μTBS) to dentin was tested in a universal testing machine. Qualitative nanoleakage analysis was performed from a central stick of each restored tooth. Degree of conversion and rate of polymerization of adhesive systems were evaluated in triplicate using real-time FT-IR. Although the inclusion of the antioxidants negatively affected the μTBS over 24 h, the antioxidant-doped adhesives maintained (SB-Vit. C, SB-Vit. E, CSE-Vit. C, EB-Querc) or increased (SB-Querc, CSE-Vit. E, CSE-Querc, EB-Vit. E, and EB-Vit. C) their μTBS during 6 months of storage. Only the μTBS of Adper Single Bond 2 dropped significantly after 6 months among the control groups. Slight changes in the nanoleakage pattern after aging were observed in all groups, except for the EB-control group, which showed a noteworthy increase in nanoleakage after 6 months, and for EB-Vit. C, which presented a remarkable decrease. A lower degree of conversion was obtained with all antioxidants in SB and EB, except for the EB-Vit. E group. Similar degrees of conversion were attained in control and experimental groups for CSE. The rate of polymerization was reduced in antioxidant-doped adhesives. The performance of antioxidants changed according to the adhesive system to which they were added, and antioxidant-doped adhesives appear to have a positive effect on the adhesive interface durability, since their bond strength obtained after 24 h was maintained or increased over time.

The influence of sulfinate agents applied as a dentin pretreatment or a mixture with multi-mode one-step self-etch adhesives (1-SEAs) on the degree of conversion (DC) and micro-tensile bond strength (μTBS) of light-cured 1-SEAs was investigated. 1-SEAs Clearfil Universal Bond Quick (UBQ) or Scotchbond Universal Adhesive (SBU) were applied to dentin in etch&rinse or self-etch mode using various application strategies: 1) no pretreatment, 2) pretreatment with 90 wt% ethanol, 3) pretreatment with a sulfinate agent Clearfil DC Activator (UDC) or Scotchbond Universal DCA (SDC), or 4) a mixture of UBQ+UDC or SBU+SDC. μTBS was measured after 24 h. Additionally, DC was measured using attenuated total reflectance Fourier-transform infrared spectroscopy. Pretreatment with sulfinate agents resulted in the highest μTBS and DC, significantly improving them especially in etch&rinse mode. The mixture of sulfinate agents with 1-SEAs was less effective. Pretreatment with ethanol significantly improved μTBS in etch&rinse mode but compromised μTBS in self-etch mode.

To evaluate the effect of dimethyl sulfoxide (DMSO) on the microtensile bond strength (µTBS), nanoleakage (NL), and degree of conversion (DC) of universal adhesives on eroded dentin. One hundred thirty-four extracted (134) human third molars were selected for the study. After the dentin surface was exposed, 128 teeth were randomly assigned to 16 experimental groups as follows: dentin surfaces (sound dentin and eroded dentin), application of DMSO (without or with the application of DMSO), and adhesive strategies (etch-and-rinse [ER] and self-etch [SE]). The universal adhesive systems iBond Universal (IBU) and Scotchbond Universal (SBU) were applied and the teeth were restored using a resin composite. After 24 h in distilled water at 37°C, the samples were sectioned and evaluated for μTBS. Selected sticks from each tooth were used for evaluating NL and DC. The remaining six teeth were used to measure the thickness of the collagen layer of the artificially eroded dentin using scanning electron microscopy. Data on μTBS, NL, and DC (%) were analyzed using three-way ANOVA and Tukey's test (α = 0.05). Significantly lower μTBS (p = 0.0001) and DC (p = 0.01) were observed for eroded dentin than for sound dentin. However, a significant increase in the μTBS (p = 0.0007) and DC (p = 0.001) was observed for both substrates when DMSO was applied. Moreover, the application of DMSO decreased the concentration of silver nitrate at the bottom of the hybrid layer for both sound and eroded dentin (p = 0.002). Eroded dentin showed enlarged tubules with the presence of a collapsed collagen fibril layer approximately 5.0 ± 2.0 mm of thickness. The bonding performance of both tested universal adhesives improved on both sound and eroded dentin with DMSO pretreatment.

Tuning drug loading and release properties of diatom silica microparticles by surface modifications