Edésia Martins Barros de Sousa

Mesoporous silica/apatite nanocomposite: special synthesis route to control local drug delivery.

Synthetic hydroxyapatite is widely used in medicine and dentistry due its notable biocompatibility and bioactivity properties. The hydroxyapatite incorporation into silica has demonstrated excellent bioactivity or biodegradability, according to the content of calcium ions. Procedures to obtain ordered mesoporous silicates rely on the micelle-forming properties of a surfactant, whose chemical composition, size and concentration control the structural dimensions of the final material. This paper reports the synthesis of two types mesoporous materials: pure MCM-41 and a nanocomposite of apatite and mesoporous silica, MCM-41-HA. The samples were charged with atenolol as a model drug and in vitro release essays were carried out. The bioactivity behavior was investigated as a function of soaking time in simulated body fluid. The materials were characterized by X-ray diffraction, N2 adsorption, FTIR spectroscopy, scanning electron microscopy, dispersive energies spectroscopy, and transmission electron microscopy. The influence of the release rate of atenolol molecules from pure MCM-41 mesoporous and containing hydroxyapatite was demonstrated, since it results in a very slowly drug delivery from the nanocomposite system.

Boron nitride nanotubes radiolabeled with 99mTc: Preparation, physicochemical characterization, biodistribution study, and scintigraphic imaging in Swiss mice

In the present study, boron nitride nanotubes (BNNTs) were synthesized from an innovative process and functionalized with a glycol chitosan polymer in CDTN (Centro de Desenvolvimento da Tecnologia Nuclear) laboratories. As a means of studying their in vivo biodistribution behavior, these nanotubes were radiolabeled with (99m)Tc and injected in mice. Their size, distribution, and homogeneity were determined by photon correlation spectroscopy (PCS), while their zeta potential was determined by laser Doppler anemometry. The morphology and structural organization were evaluated by scanning electron microscopy (SEM). The functionalization in the nanotubes was evaluated by thermogravimetry analysis (TGA) and Fourier transformer infrared spectroscopy. The results showed that BNNTs were obtained and functionalized successfully, reaching a mean size and dispersity deemed adequate for in vivo studies. The BNNTs were also evaluated by ex vivo biodistribution studies and scintigraphic imaging in healthy mice. The results showed that nanostructures, after 24h, having accumulated in the liver, spleen and gut, and eliminated via renal excretion. The findings from this study reveal a potential application of functionalized BNNTs as new potential drugs or radioisotope nanocarriers to be applied in therapeutic procedures.

Magnetic solid-phase extraction based on mesoporous silica-coated magnetic nanoparticles for analysis of oral antidiabetic drugs in human plasma.

In the present work, magnetic nanoparticles embedded into mesoporous silica were prepared in two steps: first, magnetite was synthesized by oxidation-precipitation method, and next, the magnetic nanoparticles were coated with mesoporous silica by using nonionic block copolymer surfactants as structure-directing agents. The mesoporous SiO2-coated Fe3O4 samples were functionalized using octadecyltrimethoxysilane as silanizing agent. The pure and functionalized silica nanoparticles were physicochemically and morphologically characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), N2 adsorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The resultant magnetic silica nanoparticles were applied as sorbents for magnetic solid-phase extraction (MSPE) of oral antidiabetic drugs in human plasma. Our results revealed that the magnetite nanoparticles were completely coated by well-ordered mesoporous silica with free pores and stable pore walls, and that the structural and magnetic properties of the Fe3O4 nanoparticles were preserved in the applied synthesis route. Indeed, the sorbent material was capable of extracting the antidiabetic drugs from human plasma, being useful for the sample preparation in biological matrices.

Boron nitride nanotubes coated with organic hydrophilic agents: Stability and cytocompatibility studies

In the present study, Boron Nitride Nanotubes (BNNTs) were synthesized and functionalized with organic hydrophilic agents constituted by glucosamine (GA), polyethylene glycol (PEG)1000, and chitosan (CH) forming new singular systems. Their size, distribution, and homogeneity were determined by photon correlation spectroscopy, while their surface charge was determined by laser Doppler anemometry. The morphology and structural organization were evaluated by Transmission Electron Microscopy. The functionalization was evaluated by Thermogravimetry analysis and Fourier Transformer Infrared Spectroscopy. The results showed that BNNTs were successfully obtained and functionalized, reaching a mean size and dispersity deemed adequate for in vitro studies. The in vitro stability tests also revealed a good adhesion of functionalized agents on BNNT surfaces. Finally, the in vitro cytocompatibility of functionalized BNNTs against MCR-5 cells was evaluated, and the results revealed that none of the different functionalization agents disturbed the propagation of normal cells up to the concentration of 50 μg/mL. Furthermore, in this concentration, no significantly chromosomal or morphologic alterations or increase in ROS (Reactive Oxygen Species) could be observed. Thus, findings from the present study reveal an important stability and cytocompatibility of functionalized BNNTs as new potential drugs or radioisotope nanocarriers to be applied in therapeutic procedures.

Synthesis, characterization, and biodistribution studies of (99m)Tc-labeled SBA-16 mesoporous silica nanoparticles.

Along with anti-cancer drug delivery researches, many efforts have been done to develop new tracers for diagnostic applications. Based on advances in molecular imaging, nanoparticles can be used to visualize, characterize and measure biological process at molecular and cellular level. Therefore, the purpose of this study was to synthesize, characterize and radiolabeled mesoporous silica nanoparticles (MSNs) for in vivo applications. The nanoparticles were synthesized, functionalized with 3-aminopropyltriethoxysilane (APTES) and then, anchored with diethylenetriaminepentaacetic acid (DTPA). Particles were physicochemical characterized by elemental analysis (CHN), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), and zeta potential, and were morphologically characterized by scanning electron microscopy (SEM), low-angle X-ray diffraction (XRD) and transmission electron microscopy (TEM) techniques. Results indicate that functionalization process was successfully achieved. Next, functionalized silica nanoparticles were radiolabeled with technetium-99m showing high radiochemical yields and high radiolabeled stability. These findings allow the use of the particles for in vivo applications. Biodistribution and scintigraphic images were carried out in healthy mice in order to determine the fate of the particles. Results from in vivo experiments showed high uptake by liver, as expected due to phagocytosis. However, particles also showed a significant uptake in the lungs, indicated by high lung-to-non-target tissue ratio. In summary, taking into account the great potential of these silica mesoporous structures to carry molecules this platform could be a good strategy for theranostic purposes.

Folate-grafted boron nitride nanotubes: Possible exploitation in cancer therapy

Boron nitride nanotubes (BNNTs) have generated considerable interest among the scientific community because of their unique physical and chemical properties. They present good chemical inertness, high thermal stability, and optimal resistance to oxidation, that make them ideal candidates for biomedical applications, in particular as nanovectors for drug, gene and protein delivery into the cells. In this study, BNNTs were prepared through a synthesis based on a chemical vapor deposition (CVD) method, and thereafter chemically functionalized with folic acid. The obtained nanostructures have been characterized by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The characterization showed efficiently functionalized BNNTs of length of about 1 μm. Furthermore, confocal laser microscopy demonstrated that our nanotubes can be fluorescently-traced under appropriate excitation. Thanks to this property, it has been possible to investigate their internalization by HeLa cells through confocal microscopy, demonstrating that the BNNT up-take clearly increases after the functionalization with folate, a result confirmed by inductively coupled plasma (ICP) assessment of boron content inside the treated cell cultures.

Characterization and catalytic activity studies of sol–gel Co–SiO2 nanocomposites

Abstract Silica embedded with transition metals exhibits adequate properties for applications in catalysis, sensors and optics. Cobalt–silica (Co–SiO 2 ) nanocomposites were prepared by the sol–gel method and thermally treated at 700, 900, 1100 and 1250 °C. Characterization of the samples was performed by XRD and BET nitrogen adsorption. The performance of the nanocomposites was investigated by catalysis reactions of oxidation. These catalysts were found to be recyclable showing a catalytic activity even after a third recovering. The results indicate that thermal treatment of sol–gel nanocomposites at temperatures higher than 900 °C is essential for the preparation of active heterogeneous catalysts.

Mesoporous silica materials functionalized with folic acid: preparation, characterization and release profile study with methotrexate

Ordered mesoporous silica materials exhibit potential features to be used as controlled drug delivery systems, including biocompatibility, textural and structural properties. In this paper, ordered mesoporous materials SBA-15, SBA-16 and MCM-41, which present different morphologies, pore sizes and array of mesopores (2D hexagonal, 3D cubic and 2D hexagonal, respectively), were synthesized, functionalized with folic acid by post-synthesis grafting and loaded with the anticancer agent methotrexate. The drug loading and its release kinetics profile were compared between all materials. The mesoporous silicas were characterized through thermogravimetric analysis, CHN elemental analysis, Fourier transform infrared spectroscopy, small-angle X-ray scattering, N2 adsorption, zeta potential, scanning electron microscopy and transmission electron microscopy in order to evaluate their physical–chemical properties. The interactions between methotrexate and the materials’ surface were systematically evaluated using X-ray photoelectron spectroscopy. The results showed the drug release kinetic might be controlled by the synthesis procedure and the degree of surface functionalization of the mesoporous silica.Graphical Abstract

An in situ synthesis of mesoporous SBA-16/hydroxyapatite for ciprofloxacin release: in vitro stability and cytocompatibility studies

The present work developed a biomaterial (HA/SBA-16) based on the growth of calcium phosphate (HA) particles within an organized silica structure (SBA-16) to evaluate its application as a drug delivery system. The samples were charged with ciprofloxacin as a model drug and in vitro release assays were carried out. The samples were characterized by elemental analysis (CHN), Fourier transform infrared spectroscopy, nitrogen adsorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), small angle X-ray scattering (SAXS) and X-ray diffraction. The results obtained by TEM, SEM and SAXS reveal a well-defined cubic arrangement of a uniform spherical mesoporous structure, an intrinsic characteristic of these materials, which indicated that SBA-16 and HA/SBA-16 could potentially encapsulate bioactive molecules by means of ordered mesopores. It was found that both surface interaction and pore volume affect the rate and amount of ciprofloxacin released from the mesoporous materials. In vitro assays were performed to evaluate the adhesion, viability, and growth behavior of human adipose tissue-derived stem cells (hADSC) on SBA-16 and HA/SBA-16 nanocomposites to verify their potential as a scaffold for application in bone–tissue engineering using MTT assay and alkaline phosphatase activity tests. The results showed that the materials are promising systems for bone repair, providing a good environment for the adhesion and proliferation of rat mesenchymal stem cells and hADSC in vitro.

Mesoporous silica SBA-16 functionalized with alkoxysilane groups: preparation, characterization, and release profile study

A mesoporous material sphere based on silica, SBA-16, was chemically modified with alkoxysilane using two different solvents: methanol and toluene. The influence of the chemical modification of the matrix on the release rate of a model drug was also studied. The structural characteristics of the materials were evaluated by small-angle X-ray diffraction, N2 adsorption, and transmission electron microscopy. The functionalization of the matrix was evaluated using thermal analysis, FTIR spectroscopy, 13C and 29Si solid-state nuclear magnetic resonance, and elemental analysis, CHN. The results show that alkoxysilane groups have been chemically bonded to silicon atoms on the surface of cubic Im3m mesoporous silica. The influence of the release rate of atenolol molecules from chemically modified mesoporous SBA-16 could be identified, since significant differences could be observed among the release patterns of the different materials.