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Purpose Compositional tailoring is gaining more attention in the development of advanced biomimetic nanomaterials. In this study, we aimed to prepare advanced multi-substituted hydroxyapatites (ms-HAPs), which show similarity with the inorganic phase of bones and might have therapeutic potential for bone regeneration. Materials Novel nano hydroxyapatites substituted simultaneously with divalent cations: Mg2+ (1.5%), Zn2+ (0.2%), Sr2+ (5% and 10%), and Si (0.2%) as orthosilicate (SiO4 4-) were designed and successfully synthesized for the first time. Methods The ms-HAPs were obtained via a wet-chemistry precipitation route without the use of surfactants, which is a safe and ecologically friendly method. The composition of synthesized materials was determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The materials were characterized by X-ray powder diffraction (XRD), FT-IR and FT-Raman spectroscopy, BET measurements and by imaging techniques using high-resolution TEM (HR-TEM), FE-SEM coupled with EDX, and atomic force microscopy (AFM). The ion release was measured in water and in simulated body fluid (SBF). Results Characterization methods confirmed the presence of the unique phase of pure stoichiometric HAP structure and high compositional purity of all synthesized nanomaterials. The doping elements influenced the crystallite size, the crystallinity, lattice parameters, morphology, particle size and shape, specific surface area, and porosity. Results showed a decrease in both nanoparticle size and crystallinity degree, coupled with an increase in specific surface area of these advanced ms-HAP materials, in comparison with pure stoichiometric HAP. The release of biologically important ions was confirmed in different liquid media, both in static and simulated dynamic conditions. Conclusion The incorporation of the four substituting elements into the HAP structure is demonstrated. Synthesized nanostructured ms-HAP materials might inherit the in vivo effects of substituting functional elements and properties of hydroxyapatite for bone healing and regeneration. Results revealed a rational tailoring approach for the design of a next generation of bioactive ms-HAPs as promising candidates for bone regeneration.

Purpose Compositional tailoring is gaining more attention in the development of advanced biomimetic nanomaterials. In this study, we aimed to prepare advanced multi-substituted hydroxyapatites (ms-HAPs), which show similarity with the inorganic phase of bones and might have therapeutic potential for bone regeneration. Materials Novel nano hydroxyapatites substituted simultaneously with divalent cations: Mg2+ (1.5%), Zn2+ (0.2%), Sr2+ (5% and 10%), and Si (0.2%) as orthosilicate (SiO44-) were designed and successfully synthesized for the first time. Methods The ms-HAPs were obtained via a wet-chemistry precipitation route without the use of surfactants, which is a safe and ecologically friendly method. The composition of synthesized materials was determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The materials were characterized by X-ray powder diffraction (XRD), FT-IR and FT-Raman spectroscopy, BET measurements and by imaging techniques using high-resolution TEM (HR-TEM), FE-SEM coupled with EDX, and atomic force microscopy (AFM). The ion release was measured in water and in simulated body fluid (SBF). Results Characterization methods confirmed the presence of the unique phase of pure stoichiometric HAP structure and high compositional purity of all synthesized nanomaterials. The doping elements influenced the crystallite size, the crystallinity, lattice parameters, morphology, particle size and shape, specific surface area, and porosity. Results showed a decrease in both nanoparticle size and crystallinity degree, coupled with an increase in specific surface area of these advanced ms-HAP materials, in comparison with pure stoichiometric HAP. The release of biologically important ions was confirmed in different liquid media, both in static and simulated dynamic conditions. Conclusion The incorporation of the four substituting elements into the HAP structure is demonstrated. Synthesized nanostructured ms-HAP materials might inherit the in vivo effects of substituting functional elements and properties of hydroxyapatite for bone healing and regeneration. Results revealed a rational tailoring approach for the design of a next generation of bioactive ms-HAPs as promising candidates for bone regeneration.

Introduction : The preparations based on hydroxyquinoline, in various combinations, are used in medicine, being shown to have an inhibitory effect against bacteria, molds, fungi, parasites, and viruses, but also having other beneficial effects mentioned in other medical conditions (anti-cancer, anti-degenerative, anti-inflammatory). Aims : In vitro susceptibility testing of microorganisms: bacteria (Gram positive and Gram negative), yeast ( Candida spp.,) and unicellular algae ( Prototheca spp.) at the preparations based on hydroxyquinoline (HQ) and its cupric derivatives deposited on hydroxyapatite (HAP). Materials and methods : There were tested microbial strains of the following genera: Escherichia , Staphylococcus , Micrococcus , Bacillus , Candida , and Prototheca . The tested products (developed in the Laboratory for Nanobiomaterials Synthesis, Center of Physical Chemistry, Faculty of Chemistry and Chemical Engineering, UBB Cluj-Napoca) were developed in three versions: 1) HQ–Cu 2+ –HAP 1 ; 2) HQ–Cu 2+ –HAP 2 ; and 3) NHQ–Cu 2+ –HAP 2 , where NHQ stands for nitro hydroxyquinoline. Determination of the inhibitory effect was conducted by diffusion technique in nutrient agar, according to CLSI 2013 standards, with necessary adaptations for testing of products made in the form of suspensions. Results : Following interpretation, it was found that the inhibition zones, arising from the antimicrobial effect of the tested products showed variability in size, depending on the test product and the microbial strain: Escherichia coli (8-10 mm), Staphylococcus sp. (17.6 - 23.2 mm), Micrococcus spp. (24.4 - 27.6 mm), Bacillus spp. (14.0 - 16.0 mm), Candida spp. (20.4 - 25.2 mm), Prototheca spp. (20.8 - 30.0 mm). From the three tested products, the best efficacy was found at the product no. 3 (NHQ – Cu 2+ – HAP 2 ), followed by no. 1 (HQ– Cu 2+ –HAP 1 ) and no. 2 (HQ–Cu 2+ –HAP 2 ). Conclusions : The inhibitory effect was bactericidal, manifested more intensively against Gram-positive bacteria, yeasts, and prototheca. Such products, prepared in the form of suspensions, may have practical application in the prevention and treatment of skin or hooves disorders. No resistance phenomena are recorded. Keywords : copper, hydroxyapatite, hydroxyquinoline, microorganisms, sensitivity.

This study reports the synthesis of new porous nanohydroxyapatites (HAPs) substituted with different Zn contents (HAP_Zn) employing calcium and zinc nitrates and diammonium hydrogen phosphate as precursors. The synthesis was conducted in the presence of a surfactant, L-asparagine, for controlling the pore size distribution and morphology of obtained nanopowders, using a co-precipitation route. Thus a new approach leading to HAP_Zn nanopowders with improved nucleation and crystallization ability was developed. After maturation treatment of dispersions and filtration, the precipitate was lyophilized and ground. Part of the samples was calcined at 300°C for 1 h. The zinc content in the nanoHAPs varies from 0.2 to 10 wt% (substitution degree of Ca by Zn from 0.3 to 15.8 mole %). XRD investigations indicated HAP as the unique phase present and the nanostructured nature of the obtained HAPs. FTIR spectra also confirmed the presence of HAP structure. TEM, SEM, and AFM images showed the morphology of the ...

Nano hydroxyapatite doped with zinc (0.2 wt%), silver (0.25 wt%) and gold (0.025 wt%), (HAP), has been obtained by an innovative wet chemical approach, coupled with a reduction process for silver and gold. The synthesized multi-substituted nano HAP was freeze-dried and calcined at 650 °C. Nano HAP has been characterized by XRD, FTIR spectroscopy and imaging techniques: TEM, SEM and AFM. Then, nano HAP was mixed with previously synthesized silver nanoparticles (AgNPs), in the amount of 9 wt%, to give a novel material (HAP-Ag). The AgNPs were prepared by the reduction of silver nitrate with glucose in alkaline medium. TEM and UV–Vis confirmed the formation of AgNPs with an average size of 12 nm. Further, organic matrix composites were obtained from a filler made of HAP and/or HAP-Ag and a mixture of monomers (such as bis-GMA and TEG-DMA), which were polymerized at various compositions in AgNPs content up to 5.4 wt%. Antibacterial activities of these composites were investigated against several different pathogenic species: Escherichia coli, Staphylococcus aureus, Staphylococcus spp., Bacillus cereus, and Candida albicans, using the Kirby–Bauer disk-diffusion method. Antibacterial activities are enhanced with increasing of silver content within composites. These effects clearly reveal that AgNPs can be effectively utilized in combination with multi-substituted HAP and polymeric matrix, both used as carriers, in order to improve their efficiency against various pathogenic species. These composites can be considered a promising antimicrobial material for coating of orthopedic and dental implants or used as bone cements in surgical applications.

Although total joint replacement surgery has become common in recent years, problems due to bacterial infection remain a significant complication following this procedure. One approach in our study was to obtain a self-cured bone cement based on hydroxyapatite with nanosilver (Hap-Ag) and ZrO2 and polymer matrix based on 2,2-bis[4-(2-hydroxy-3-methacryloyloxypropoxy)-phenyl]propane/triethyleneglycol dimethacrylate. New materials were tested for: in vitro silver release, compressive strength (CS), compressive modulus (CM), and radiopacity. In vitro silver release increased in time and depended of silver content in cement. The highest silver release was registered for the cement with 1.26 wt% silver content. The results reveal that the CS for bone cement was between 133.37 and 146.70 MPa and CM was between 1.68 and 1.82 GPa (p > 0.05). A slow increasing of CM was registered for samples with 1.5/1 powder/liquid ratio. Addition of nanosilver and ZrO2 increased radiopacity of experimental bone cement.

Aurora Mocanu,1 Roxana Diana Pasca,1 Gheorghe Tomoaia,2 Corina Garbo,1 Petre T Frangopol,1 Ossi Horovitz,1 Maria Tomoaia-Cotisel11Chemical Engineering Department, Babes-Bolyai University, 2Orthopedic Department, Iuliu Hatieganu University of Medicine and Pharmacy, Cluj-Napoca, RomaniaAbstract: Silver nanoparticles (AgNPs) were prepared in aqueous colloid dispersions by the reduction of Ag+ with glucose in alkaline medium. Tetraethyl orthosilicate and l-asparagine were added as stabilizers of NPs. The AgNPs were characterized, and their interaction with three local anesthetics (procaine, dibucaine, or tetracaine) was investigated. Optical spectra show the characteristic absorption band of AgNPs, due to surface plasmon resonance. Modifications in the position and shape of this band reflect the self-assembly of metal NPs mediated by anesthetic molecules and the progress in time of the aggregation process. Zeta-potential measuring was applied in order to characterize the electrostatic stability of the NPs. The size and shape of the AgNPs, as well as the features of the assemblies formed by their association in the presence of anesthetics, were evidenced by transmission electron microscopy images. Atomic force microscopy images showed the characteristics of the films of AgNPs deposited on glass support. The effect of the anesthetics could be described in terms of electrostatic forces between the negatively charged AgNPs and the anesthetic molecules, existing also in their cationic form at the working pH. But also hydrophobic and hydrogen bonding interactions between the coated nanoparticles and anesthetics molecular species should be considered.Keywords: self-assembled nanostructures, UV-vis spectra, TEM, AFM, zeta potential