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1.
Steroids ; 187: 109099, 2022 11.
Artigo em Inglês | MEDLINE | ID: mdl-35970223

RESUMO

Structural modification of the phenolic A-ring of estrogens at C-2 and/or C-3 significantly reduces or eliminates the hormonal effects of the compounds, thus the incorporation of other pharmacophores into these positions can provide biologically active derivatives suitable for new indications, without possessing unwanted side effects. As part of this work, A-ring integration of estradiol with chalcones and flavones was carried out in the hope of obtaining novel molecular hybrids with anticancer action. The syntheses were performed from 2-acetylestradiol-17ß-acetate which was first reacted with various (hetero)aromatic aldehydes in a pyrrolidine-catalyzed reaction in DMSO. The chalcones thus obtained were then subjected to oxidative cyclization with I2 in DMSO to afford estradiol-flavone hybrids in good yields. All newly synthesized derivatives were tested in vitro for cytotoxicity on human malignant cell lines of diverse origins as well as on a non-cancerous cell line, and the results demonstrated that estradiol-flavone hybrids containing a structure-integrated flavone moiety were the most active and cancer cell-selective agents. The minimal inhibitory concentration values (IC50) were calculated for selected compounds (3c, 3d and 3e) and their apoptosis inducing capacity was verified by RT-qPCR (real-time quantitative polymerase chain reaction). The results suggest an important structure-activity relationship regarding estradiol-flavone hybrids that could form a promising synthetic platform and rationale for future drug developments.


Assuntos
Antineoplásicos , Chalcona , Chalconas , Flavonas , Aldeídos , Antineoplásicos/química , Antineoplásicos/farmacologia , Linhagem Celular Tumoral , Proliferação de Células , Chalcona/química , Chalcona/farmacologia , Chalconas/química , Dimetil Sulfóxido/farmacologia , Ensaios de Seleção de Medicamentos Antitumorais , Estradiol/farmacologia , Estrogênios/farmacologia , Flavonas/química , Flavonas/farmacologia , Humanos , Estrutura Molecular , Pirrolidinas , Relação Estrutura-Atividade
2.
Materials (Basel) ; 14(17)2021 Aug 27.
Artigo em Inglês | MEDLINE | ID: mdl-34500969

RESUMO

The synthesis of the copper-poor and aluminum-rich layered double hydroxides (LDHs) of the CuAl4 type was optimized in detail in this work, by applying an intense mechanochemical treatment to activate the gibbsite starting reagent. The phase-pure forms of these LDHs were prepared for the first time; using copper nitrate and perchlorate salts during the syntheses turned out to be the key to avoiding the formation of copper hydroxide sideproducts. Based on the use of the optimized syntheses parameters, the preparation of layered triple and multiple hydroxides was also attempted using Ni(II), Co(II), Zn(II) and even Mg(II) ions. These studies let us identify the relative positions of the incorporating cations in the well-known selectivity series as Ni2+ >> Cu2+ >> Zn2+ > Co2+ >> Mg2+. The solids formed were characterized by using powder X-ray diffractometry, UV-Vis diffuse reflectance spectroscopy, Fourier-transform infrared spectroscopy, thermogravimetric analysis and scanning electron microscopy. The catalytic potential of the samples was investigated in carbon monoxide oxidation reactions at atmospheric pressure, supported by an in situ diffuse reflectance infrared spectroscopy probe. All solids proved to be active and the combination of the nickel and cobalt incorporation (which resulted in a NiCoAl8 layered triple hydroxide) brought outstanding benefits regarding low-temperature oxidation and increased carbon monoxide conversion values.

3.
Nanomaterials (Basel) ; 10(10)2020 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-33019625

RESUMO

In the present work, visible light active bismuth oxyiodide (BiOI) was immobilized on a commercial, non-conductive support (an Al2O3 based ceramic paper) using a novel two-step spray coating technique and investigated with different characterization methods (e.g., SEM, Raman, XPS). Our main goal was to eliminate the separation costs after the photocatalytic measurement and investigate the chemical relevance and opportunity to use this technique in the industry. Our as-prepared uniform BiOI layer had similar properties to the well-known reference BiOI powder. The Raman and XPS measurements confirmed that the enriched amount of the surface iodine defined the color and as well the band gap of the BiOI layer. The durable BiOI layers have prominent photocatalytic activity under UV and visible light irradiation as well. The scale-up procedure proved that the designed BiOI coated paper was reusable and potentially applicable in the industry by straightforward scale-up, which is due to the elaborated non-conventional BiOI coverage estimation method. This immobilization technique could open several opportunities for immobilizing many other visible light active photocatalysts with simple materials and low cost.

4.
Molecules ; 25(20)2020 Oct 14.
Artigo em Inglês | MEDLINE | ID: mdl-33066653

RESUMO

In the present work, the structure and thermal stability of Ca-Al mixed-metal compounds, relevant in the Bayer process as intermediates, have been investigated. X-ray diffraction (XRD) measurements revealed the amorphous morphology of the compounds, which was corroborated by SEM-EDX measurements. The results of ICP-OES and UV-Vis experiments suggested the formation of three possible ternary calcium aluminum heptagluconate (Ca-Al-Hpgl) compounds, with the formulae of CaAlHpgl(OH)40, Ca2AlHpgl2(OH)50 and Ca3Al2Hpgl3(OH)90. Additional IR and Raman experiments revealed the centrally symmetric arrangement of heptagluconate around the metal ion. The increased thermal stability was demonstrated by thermal analysis of the solids and confirmed our findings.


Assuntos
Alumínio/química , Cálcio/química , Gluconatos/química , Cristalografia por Raios X , Microscopia Eletrônica de Varredura , Estrutura Molecular , Espectrometria por Raios X , Espectrofotometria Infravermelho , Espectroscopia de Infravermelho com Transformada de Fourier , Análise Espectral Raman , Temperatura , Termogravimetria
5.
Molecules ; 25(20)2020 Oct 20.
Artigo em Inglês | MEDLINE | ID: mdl-33092291

RESUMO

In the present study, additive-free, pH-driven, hydrothermal crystallization was used to obtain shape-tailored monoclinic BiVO4 photocatalysts. The as-prepared BiVO4 products were systematically characterized, uncovering their crystallographic, morphologic and optical properties, while their applicability was verified in the visible light-driven photodegradation of oxalic acid and rhodamine B. Monoclinic clinobisvanite was obtained in most cases, with their band gap values located between 2.1 and 2.4 eV. The morphology varied from large, aggregated crystals, individual microcrystals to hierarchical microstructures. It was found that the degradation efficiency values obtained in the case of oxalic acid were directly related to the presence of (040) crystallographic plane, while the degradation of rhodamine B was partially independent by the presence of this structural feature. The importance of (040) crystallographic plane was also demonstrated via the reduction of Cu2+ to Cu, by analyzing the Raman spectra of the Cu containing samples, the mean primary crystallite size of Cu and Cu content. Furthermore, the presence of (040) crystallographic plane was directly proportional with the hydrodynamic properties of the powders as well.


Assuntos
Bismuto/química , Fotólise/efeitos da radiação , Semicondutores , Vanadatos/química , Catálise/efeitos da radiação , Cristalização , Luz , Vanadatos/síntese química , Poluentes Químicos da Água/química
6.
Nanoscale ; 7(13): 5776-86, 2015 Mar 19.
Artigo em Inglês | MEDLINE | ID: mdl-25757557

RESUMO

One of the most fundamental aspects of the heterogeneous catalysis field is the manipulation of the catalysts' activity. In photocatalysis this is carried out by maximizing the right crystal plane of a semiconductor oxide. Until now, most of the papers have achieved this by a combination of different oxides, with noble metals and sometimes with carbon nanomaterials. In this work MWCNTs (multiwalled carbon nanotubes) were applied as "crystallization promoters" in a very simple, safe, one-step hydrothermal method. By this method TiO2 nano/micro crystals with exposed {001} facets were obtained in the first step. The next episode in the crystal manipulation "saga" was the modification of the (001) crystallographic plane's structure by creating ordered/own faceted "crystallographic holes". These elements are capable of further enhancing the obtained activity of titania microcrystals to a higher extent, as shown by the UV driven photocatalytic phenol degradation experiments. The appearance of the holes was "provoked" by simple calcination and their presence and influence were demonstrated by XPS and HRTEM.

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