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Minimizing the risk of secondary caries in dentistry is achieved by using adhesive systems that provide a strong bond between the natural hard tissue and the restorative material. Evaluating the effectiveness of these systems requires studying both their interaction with dentin and enamel and their behavior in environments with varying acidity. In this work, the interaction of a reactive monomer, 4-methacryloxyethyl trimellitic anhydride (4-META), used in adhesive systems with both dentin-like hydroxyapatite (HA) and hydroxyapatite ceramics, was investigated. Kinetic studies showed that under experimental conditions, 4-META was hydrolyzed and amorphized. Dentin-like HA possessed greater adsorption capacity to 4-META than ceramic HA. Immersion of HA into a solution of 4-META led to formation of an acidic calcium phosphate phase over time in both systems. Studies on the solubility of the synthetic nanosized hydroxyapatite and its derivative with 4-META in 0.1 mol/L lactic acid, also containing CaCl2, Na2HPO4, and NaF (pH 4.5), and in distilled water (pH 6.3) indicated the occurrence of dissolution, complexation, and crystallization processes, causing changes in the liquid and solid phases. The total Ca2+ concentration upon dissolution of hybrid HA-4-META in a lactic acid solution was three times lower than the total Ca2+ concentration upon dissolution of pure HA. This suggested that 4-META-treated dentin-like surfaces demonstrate greater resistance to dissolution in acidic environments compared to untreated surfaces, highlighting the potential for these hybrids in dental applications.

Hybrid materials based on calcium phosphates and synthetic polymers can potentially be used for caries protection due to their similarity to hard tissues in terms of composition, structure and a number of properties. This study is focused on the biomimetic synthesis of hybrid materials consisting of hydroxiapatite and the zwitterionic polymers polysulfobetaine (PSB) and polycarboxybetaine (PCB) using controlled media conditions with a constant pH of 8.0–8.2 and Ca/P = 1.67. The results show that pH control is a dominant factor in the crystal phase formation, so nano-crystalline hydroxyapatite with a Ca/P ratio of 1.63–1.71 was observed as the mineral phase in all the materials prepared. The final polymer content measured for the synthesized hybrid materials was 48–52%. The polymer type affects the final microstructure, and the mineral particle size is thinner and smaller in the synthesis performed using PCB than using PSB. The final intermolecular interaction of the nano-crystallized hydroxyapatite was demonstrated to be stronger with PCB than with PSB as shown by our IR and Raman spectroscopy analyses. The higher remineralization potential of the PCB-containing synthesized material was demonstrated by in vitro testing using artificial saliva.

The chemical and structural similarity of calcium orthophosphates to hard tissues in the human body makes them suitable as biomaterials for bone implants, cements, injection systems, etc., for bone regeneration and reconstruction. Tetracalcium phosphate (Ca4(PO4)2O, TTCP) is a promising component for such biomaterials due to its high calcium content and alkaline nature. The former makes it suitable for promoting mineralization, while the latter supports neutralization of the acidic environment, helping to prevent inflammation and improve the biocompatibility of the materials. However, it is the least used calcium orthophosphate due to the difficulties in its synthesis. This study examines the effect of high-energy mechanochemical activation on the phase evolution, particle morphology, and thermal behaviour of equimolar mixtures of Ca(OH)2 and CaHPO4, with the aim of optimizing precursor conditions for the synthesis of (TTCP)-rich ceramic materials. The results demonstrate that mechanochemical activation effectively induces structural disorder, promotes the formation of amorphous and nanocrystalline phases, and facilitates subsequent phase transitions upon calcination. The combined use of solid-state NMR, XRD, TEM, and thermal analysis provides a comprehensive understanding of the transformation pathways. Ultimately, 24 h of activation under the experimental conditions was identified as optimal for producing a precursor with a favorable phase composition for obtaining TTCP-rich ceramic materials after calcination at 1350 °C.

Simulated body fluid (SBF) and artificial saliva (AS) are used in biomedical and dental research to mimic the physiological conditions of the human body. In this study, the biomimetic precipitation of double-doped amorphous calcium phosphate in SBF and AS are compared by thermodynamic modelling of chemical equilibrium in the SBF/AS-CaCl2-MgCl2-ZnCl2-K2HPO4-H2O and SBF/AS-CaCl2-MgCl2-ZnCl2-K2HPO4-Glycine/Valine-H2O systems. The saturation indices (SIs) of possible precipitate solid phases at pH 6.5, close to pH of AS, pH 7.5, close to pH of SBF, and pH 8.5, chosen by us based on our previous experimental data, were calculated. The results show possible precipitation of the same salts with almost equal SIs in the two biomimetic environments at the studied pHs. A decrease in the saturation indices of magnesium and zinc phosphates in the presence of glycine is a prerequisite for reducing their concentrations in the precipitates. Experimental studies confirmed the thermodynamic predictions. Only X-ray amorphous calcium phosphate with incorporated Mg (5.86–8.85 mol%) and Zn (0.71–2.84 mol%) was obtained in the experimental studies, irrespective of biomimetic media and synthesis route. Solid-state nuclear magnetic resonance (NMR) analysis showed that the synthesis route affects the degree of structural disorder of the precipitates. The lowest concentration of dopant ions was obtained in the presence of glycine. Further, the behaviour of the selected amorphous phase in artificial saliva was studied. The dynamic of Ca2+, Mg2+, and Zn2+ ions between the solid and liquid phases was monitored. Both direct excitation 31P NMR spectra and 1H-31P CP-MAS spectra proved the increase in the nanocrystalline hydroxyapatite phase upon increasing the incubation time in AS, which is more pronounced in samples with lower additives. The effect of the initial concentration of doped ions on the solid phase transformation was assessed by solid-state NMR.

The preparation of specially doped calcium phosphates (CaPs) is receiving a great deal of attention from researchers due to CaPs’ enhanced capabilities for application in medicine. Complexation and precipitation in a complicated electrolyte system including simulated body fluids that are enriched with Mg2+ and Zn2+ ions and modified with glycine, alanine and valine were first evaluated using a thermodynamic equilibrium model. The influence of the type and concentration of amino acid on the incorporation degree of Mg and Zn into the solid phases was predicted. Experimental studies, designed on the basis of thermodynamic calculations, confirmed the predictions. Amorphous calcium phosphates double-doped with Mg and Zn were biomimetically precipitated and transformed into Mg, Zn-β—tricalcium phosphates (TCP) upon calcination. The Rietveld refinement confirmed that Mg2+ and Zn2+ substituted Ca2+ only at the octahedral sites of β-TCP, and in some cases, fully displacing the Ca2+ from them. The resulting Mg, Zn-β–TCP can serve as a reservoir for Mg and Zn ions when included in the formulation of a biomaterial for bone remodeling. The research conducted reveals the effect of combining mathematical models with experimental studies to pre-evaluate the influence of various additives in the design of materials with predetermined properties.

The inorganic chemical species in Maresh and Luda Yana rivers affected by the Cu- Mo Asarel-Medet mine, Bulgaria were determined during a low-flow and a high-flow period. The mining activities, the weathering and the oxidation processes strongly influenced the physicochemical processes in the whole water system. The main pollution source was a small lake receiving the acid effluents of the mining activities. High levels of SO₄ ² ⁻ , Cu, Mg, Al, Mn and Fe were determined at the mining polluted and affected stations. Cu² ⁺ and CuCO₃ ⁰ species (1:1) were present in the reference waters and Cu² ⁺ and CuSO₄ ⁰ species (1:1) in the polluted and affected waters; Cu² ⁺ species was dominating downstream. Me² ⁺ followed by [graphic removed] (Me = Mn, Zn, Cd and Pb), [graphic removed] and [graphic removed] species as well as [graphic removed] , [graphic removed] , [graphic removed] , [graphic removed] were prevailing in the system. [graphic removed] and [graphic removed] (Me = Fe, Al), [graphic removed] (Me = Zn, Cd and Pb), [graphic removed] (Me = Zn, Cd) and [graphic removed] species polluted and affected waters. The major elements K and Na were mainly Me ⁺ species, whereas Ca and Mg were Me² ⁺ and [graphic removed] species in different ratios. The concentration of concentration of [graphic removed] , [graphic removed] and [graphic removed] species as well as complex phosphorous species such as H₂ [graphic removed] , [graphic removed] , [graphic removed] , [graphic removed] , [graphic removed] and [graphic removed] were also calculated. The trace element concentrations decreased downstream due to dilution, sorption processes and precipitation, but the percentage of free metal species, which are more toxic, increased. An exception was iron and aluminum of which the dominant hydroxy colloidal and sulphate species were easily incorporated into the suspended phase.

Bacterial infection is one of the most common and harmful medical issues following the implantation of materials and devices in the body leading to antibiotic resistance of diverse bacterial strains. In this work, a novel approach is presented combining adopted laser-based patterning method in addition to doping (Mg and Zn) metal ions to prepare calcium phosphate ceramic substrate, applicable in medicine, with enhanced surface antimicrobial characteristics. The preparation of tablets containing Mg (8.44 mol%) and Zn (2.63 mol%) β-tricalcium phosphate involved biomimetic precipitation of amorphous calcium phosphate in media of simulated body fluid enriched with Mg2+ and Zn2+ ions as well as the presence of valine as an organic additive, followed by step-wise calcination up to 1000 °C. The results from laser processing showed formation of deeper patterns with increased surface roughness (from 4.9 µm to 9.4 µm) as laser power and velocity increase, keeping constant the hatch sizes of 50 µm. The textured surfaces consist of peaks and valleys arrangement that change the morphology of Escherichia coli cells and decrease of cell viability. Our study reveals the possibilities of the application of ultra-short laser radiation as a potential alternative therapy for controlling the antimicrobial effect of the ceramic surface.

Biomacromolecules control mineral formation during the biomineralization process, but the effects of the organic components’ functionality on the type of mineral phase is still unclear. The biomimetic precipitation of calcium phosphates in a physiological medium containing either polycarboxybetaine (PCB) or polysulfobetaine (PSB) was investigated in this study. Amorphous calcium phosphate (ACP) or a mixture of octacalcium phosphate (OCP) and dicalcium phosphate dihydrate (DCPD) in different ratios were identified depending on the sequence of initial solution mixing and on the type of the negative functional group of the polymer used. The more acidic character of the sulfo group in PSB than the carboxy one in PCB determines the dominance of the acidic solid phases, namely, an acidic amorphous phase or DCPD. In the presence of PCB, the formation of ACP with acicular particles arranged in bundles with the same orientation was observed. A preliminary study on the remineralization potential of the hybrid material with the participation of PSB and a mixture of OCP and DCPD did not show an increase in enamel density, contrary to the materials based on PCB and ACP. Moreover, the latter showed the creation of a newly formed crystal layer similar to that of the underlying enamel. This defines PCB/ACP as a promising material for enamel remineralization.

The assessment of the ecological status of natural surface water, in terms of dominant trace metals, within an area subject to various sources of pollution including a non-ferrous metal ore mining, such as the West Rhodope Mountain, Bulgaria, is significant. The present study estimates the ecological status of river body waters at industrial areas of the West Rhodope Mountain, Bulgaria, simultaneously evaluating the possibility of state forecasting, together with assessing the potential risks, through the study of scenarios focusing on (i) possible variations of physicochemical parameters such as pH, concentration levels of trace metals, sulphates, and dissolved organic carbon (DOC) of surface water and (ii) consideration of potential spontaneous precipitation reactions in the studied waters. The ecological status of river body waters was assessed through a combination of experimental field, laboratory, and computational techniques. Al, Mn, Zn, and Pb were found to be the dominant pollutants with a variety of chemical species and distribution. The most significant difference characterizing the chemical species distribution in light of total spontaneous crystallization in the systems was found for Pb, followed by Zn and Mn, with the differences being more significant at lower trace metal levels. The calculated species were discussed on the basis of HSAB (hard and soft acids and bases) principle.

This research compares the water quality in four river bodies passing through different cities in Bulgaria. An eco-chemical approach was applied including physicochemical and analytical measurements, as well as calculation of different pollution indices and the distribution of the element species as an indicator of their bioavailability. The results from analytical measurements and calculated pollution indices show that all the studied water bodies were polluted regarding Р-РО4\", N-NHu·, Mn, and Pb. The highest values were measured in the Struma River, which is the result of both natural origin, due to the presence of coal mines, and the unsustainable management of mining and metallurgy activities in the past. The second most polluted is the Iskar River near Sofia city, mainly a consequence of the increased population in recent years. Thermodynamically calculated species of trace metals show that free Mn?\" ions dominate in all rivers being highest in Struma river. They are dangerous for aquatic fauna as free metal ions easily interact with ligands of organic compounds found in the bloodstream and/or within organs. Free ions are also calculated for Zn, but it is less dangerous because its content is significantly less. It was found only at single stations in the Maritsa and Danube rivers. Cu and Pb are potentially the riskiest elements for plants as their dominant organometallic species are easily accumulated by them. Regarding Al, its dominant hydroxy species are a prerequisite for the precipitation of Al(OH); and the self-purification of waters.