Study of a series of cobalt(II) sulfonamide complexes: Synthesis, spectroscopic characterization, and microbiological evaluation against M. tuberculosis. Crystal structure of [Co(sulfamethoxazole)2(H 2O)2]·H2O

Nowadays, the research for new and better antimicrobial compounds is an important field due to the increase of immunocompromised patients, the use of invasive medical procedures and extensive surgeries, among others, that can affect the incidence of infections. Another big problem associated is the occurrence of drug-resistant microbial strains that impels a ceaseless search for new antimicrobial agents. In this context, a series of heterocyclic- sulfonamide complexes with Co(II) was synthesized and characterized with the aim of obtaining new antimicrobial compounds. The structural characterization was performed using different spectroscopic methods (UV-Vis, IR, and EPR). In spite of the fact that the general stoichiometry for all the complexes was Co(sulfonamide)2·nH2O, the coordination atoms were different depending on the coordinated sulfonamide. The crystal structure of [Co(sulfamethoxazole)2(H2O)2]·H 2O was obtained by X-ray diffraction showing that Co(II) is in a slightly tetragonal distorted octahedron where sulfamethoxazole molecules act as a head-to-tail bridges between two cobalt atoms, forming polymeric chains. Besides, the activity against Mycobacterium tuberculosis, one of the responsible for tuberculosis, and the cytotoxicity on J774A.1 macrophage cells were evaluated. © 2012 Elsevier B.V. All rights reserved.

Micro-raman spectroscopic characterization of a CR-39 detector

Characterization by micro-Raman spectroscopy of polymeric materials used as nuclear track detectors reveals physico-chemical and morphological information on the material's molecular structure. In this work, the nuclear track detector poly(allyl diglycol carbonate), or Columbia Resin 39 (CR-39), was characterized according to the fluence of alpha particles produced by a 226Ra source and chemical etching time. Therefore, damage of the CR-39 chemical structure due to the alpha-particle interaction with the detector was analyzed at the molecular level. It was observed that the ionization and molecular excitation of the CR-39 after the irradiation process entail cleavage of chemical bonds and formation of latent track. In addition, after the chemical etching, there is also loss of polymer structure, leading to the decrease of the group density C-O-C (∼888 cm-1), CH=CH (∼960 cm -1), C-O (∼1110 cm-1), C-O-C (∼1240 cm -1), C-O (∼1290 cm-1), C-O (∼1741 cm -1), -CH2- (∼2910 cm-1), and the main band -CH2- (∼2950 cm-1). The analyses performed after irradiation and chemical etching led to a better understanding of the CR-39 molecular structure and better comprehension of the process of the formation of the track, which is related to chemical etching kinetics. Copyright © 2013 Society for Applied Spectroscopy.

A polymeric europium complex with the ligand thiophene-2-carboxylic acid: Synthesis, structural and spectroscopic characterization

A polymeric complex [Eu(α-tpc)3(α-Htpc) 2]n and its characterization by single crystal X-ray and thermal analysis, infrared and photoluminescence spectroscopies are described. The compound crystallizes in the monoclinic Cc space group. The asymmetric unit is formed from a europium ion bonded to one carboxyl oxygen of five different thiophene carboxylic moieties. Three of these moieties are deprotonated and bridge between neighboring europium ions giving rise to an infinite polymer along the c axis. Besides the europium characteristic emission lines, the emission spectra show unambiguously the crystal size effect on the 5D0 → 7F0 transition. The complex thermal decomposition at 220 C leads to a stable luminescent complex in which the 5D0 → 7F4 transition reveals a monomeric characteristic. The Judd-Ofelt intensity parameters to the polymeric and the monomeric compound with the same ligand and coordination number were compared. © 2013 Published by Elsevier Ltd.

Mono- and dinuclear palladium(II) compounds containing N,S donor ligands - Synthesis, characterization and thermal behavior

Synthesis, spectroscopic characterization and thermal analysis of the compounds [Pd-2(dmba)(2)(mu-NCO)(mu-2-qnS)] (1), [Pd-2(dmba)(2)(mu-NCO)(mu-8-qnS)] (2), [Pd(2-qnS)(2)] (3) and [Pd(8-qn(S))2] (4) (dmba=N,N-dimethylbenzylamine; 2-qnS=2-quinolinethiolate; 8-qnS=8-quinolinethiolate) are described. The thermal decomposition of these compounds occurs in four consecutive steps and the final decomposition products were identified as Pd(0) by X-ray powder diffraction. The thermal stability order of the complexes is 4 > 3 > 1 > 2.

Thermal and spectroscopic investigation on N,N-dimethylbenzylamine based cyclopalladated compounds containing isonicotinamide

Synthesis, spectroscopic characterization and thermal analysis of the [Pd(dmba)(Cl)(iso)] (1), [Pd(dmba)(NCO)(iso)] (2), [Pd(dmba)(N(3))(iso)] (3) and [Pd(dmba)(Br)(iso)] (4) (dmba = N,N'-dimethylbenzylamine; iso = isonicotinamide) compounds are described in this work. The complexes were investigated by infrared spectroscopy (IR), differential thermal analysis (DTA) and thermogravimetry (TG) and the residues of the thermal decomposition were identified as Pd(o) by X-ray powder diffraction. The thermal stability order of the complexes varied as [Pd(dmba)(Cl)(iso)] (1) > [Pd(dmba)(Br)(iso)] (4) > [Pd(dmba)(NCO)(iso)] (2) > [Pd(dmba)(N(3))(iso)] (3).

Expression, purification and spectroscopic analysis of an HdrC: An iron-sulfur cluster-containing protein from Acidithiobacillus ferrooxidans

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Coordinative versatility of a Schiff base containing thiophene: Synthesis, characterization and biological activity of zinc(II) and silver(I) complexes

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Thermal and spectroscopic studies of the antioxidant food additive propyl gallate

Literature mentions propyl gallate (PG) as a non-toxic synthetic antioxidant that can be used as a food additive due to its high tolerance to heat. It is important to understand the thermal properties and to identify the decomposition products of this substance, since it has been reported to be thermally stable at temperatures as high as 300 °C. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), differential scanning calorimetry-photovisual (DSC-photovisual), coupled thermogravimetry-infrared spectroscopy (TG-FTIR) analyses and spectroscopic techniques were used to study the food additive PG. The TG-DTA curves, which were performed with the aid of DSC-photovisual, provided information concerning the thermal stability and decomposition profiles of the compound. From the TG-FTIR coupled techniques, it was possible to identify n-propanol as a possible volatile compound released during the thermal decomposition of the antioxidant. A complete spectroscopic characterization in the ultraviolet, visible, near and middle infrared regions was performed in order to understand the spectroscopic properties of PG.

Synthesis, spectral and thermal studies on pyrazolate-bridged palladium(II) coordination polymers

Synthesis, spectroscopic characterization and thermal behavior of pyrazolate-bridged palladium complexes [Pd(mu-Pz)(2)](n) (1), [Pd(mu-mPz)(2)](n) (2), [Pd(mu-dmPz)(2)](n) (3), [Pd(mu-IPz)(2)](n) (4) {pyrazolate (Pz(-)), 4-methylpyrazolate (mPz(-)), 3,5-dimethylpyrazolate (dmPz(-)), 4-iodopyrazolate (IPz(-))} have been described in this work. The exobidentate coordination mode of pyrazolato ligands in 1-4 was inferred on basis of IR spectroscopic evidences. TG investigations indicated that the introduction of substituents at the 4 position in the pyrazolyl moiety into coordination polymers do not affect significantly their thermal stability, whereas at the 3 and 5 position reduced the stability of the main chain. Metal palladium was the final product of the thermal decompositions, which was identified by X-ray powder diffraction.

Assessment of maturity degree of composts from domestic solid wastes by fluorescence and fourier transform infrared spectroscopies

Methods of assessment of compost maturity are needed so the application of composted materials to lands will provide optimal benefits. The aim of the present paper is to assess the maturity reached by composts from domestic solid wastes (DSW) prepared under periodic and permanent aeration systems and sampled at different composting time, by means of excitation-emission matrix (EEM) fluorescence spectroscopy and Fourier transform infrared spectroscopy (FT-IR). EEM spectra indicated the presence of two different fluorophores centered, respectively, at Ex/Em wavelength pairs of 330/425 and 280/330 nm. The fluorescence intensities of these peaks were also analyzed, showing trends related to the maturity of composts. The contour density of EEM maps appeared to be strongly reduced with composting days. After 30 and 45 days of composting, FT-IR spectra exhibited a decrease of intensity of peaks assigned to polysaccharides and in the aliphatic region. EEM and FT-IR techniques seem to produce spectra that correlate with the degree of maturity of the compost. Further refinement of these techniques should provide a relatively rapid method of assessing the suitability of the compost to land application.

Thermal studies on nickel(II) 4-iodopyrazole complexes

This work describes the synthesis, IR and UV-Vis spectroscopic characterization as well the thermal behavior of the [NiCl2(HIPz)(4)]center dot C3H6O (1), [Ni(H2O)(2)(HIPz)(4)](NO3)(2) (2), [Ni(NCS)(2)(HIPz)(4)] (3) and [Ni(N-3)(2)(HIPz)(4)] (4) (HIPz = 4-iodopyrazole) pyrazolyl complexes. TG experiments reveal that the compounds 1-4 undergo thermal decomposition in three or four mass loss steps yielding NiO as final residue, which was identified by X-ray powder diffraction.

Luminescent properties of yttrium diphenylphosphinate activated by europium

The synthesis and spectroscopic characterization of yttrium diphenylphosphinates doped with europium are reported. The purity of all samples was confirmed by carbon and hydrogen micro analysis, thermal analysis, IR vibrational spectroscopy, and X-ray diffraction. Luminescence spectra indicated the presence of two or more symmetry centers. The dynamic luminescence measurements suggested that one symmetry site presented an inversion center, while the others had lower symmetry. The average quantum yield of Eu3+ emission in the yttrium, matrices was 60%. (c) 2005 Elsevier B.V. All rights reserved.

Thermal study of mononuclear Pd(II) complexes of the type [Pd(X)(2)(Rtu)(PPh3)] (X = Cl, SCN; Rtu = N-methylthiourea, N-phenylthiourea)

The synthesis, spectroscopic characterization, and thermal analysis of the compounds [Pd(X)(2)(mtu)(PPh3)] (X = Cl- (1), SCN- (2); mtu = N-methylthiourea; PPh3 = triphenylphosphine) and [Pd(X)(2)(phtu)(PPh3)] (X = Cl- (3), SCN- (4); phtu = N-phenylthiourea) are described. The thermal decomposition of the compounds occurs in two, three, or four stages and the final decomposition products were identified as Pd-0 by X-ray powder diffraction. The thermal stability order of the complexes is 4 > 3 > 2 > 1.

Research of new mixed-chelate copper complexes with quinoxaline N 1,N 4,-dioxide derivatives and alanine as ligands, potential antimycobacterial agents

Three new mixed-chelate copper complexes with 3-aminoquinoxaline-2-carbonitrile N 1,N 4-dioxide derivatives and alanine as ligands were synthesized in solid state. The spectroscopic characterization (FTIR, EPR, UV-Vis) showed that copper coordinated through the amine and the N-oxide groups of the quinoxaline derivatives and the amine and carboxylate moieties from alanine forming a dimeric species. The tree complexes showed in vitro activity against M. tuberculosis H 37Rv (ATCC 27294) similar to that of ethambutol while they are inactive against E. coli and S. aureus.

N,N,N-trimethyl chitosan nanoparticles as a vitamin carrier system

There is considerable interest in incorporating stabilized vitamins into biopolymeric nanoparticles, especially in the development of carriers and active systems for pharmaceutical and food applications. Amongst biopolymer, chitosan is highly desirable owing to its good biocompatibility, biodegradability and ability to be chemically modified. In this paper, nanoparticles from three kinds of water-soluble derivative chitosan (N,N,N-trimethyl chitosan, TMC) have successfully been synthesized by ionic gelation with tripolyphosphate (TPP) anions. Combinations of concentrations of TMC and TPP have resulted in nanoparticles with varying sizes for which the capability for loading with vitamins was investigated. Zeta potential measurement and particle size analysis demonstrated that the size of the nanoparticles wasoptimized (196±8nm) when the lowest TMC and TPP amounts were used, i.e., 0.86mgmL -1 and 0.114mgmL -1 respectively. As the TMC and/or the TPP concentrations increase, the resulting size of the nanoparticles increases considerably. Three different vitamins (B9, B12 and C) were tested as additives and the final system characterized in relation to size, morphology, spectroscopic and zeta potential properties. In general, the incorporation of vitamins increased all the TMC-TPP original nanoparticle sizes, reaching a maximum diameter of 534±20nm when loaded with vitamin C. The presence of vitamins also decreases the zeta potential, with one exception observed when using vitamin C. The preliminary results of this study suggested that all TMC/TPP nanoparticles can be successfully used as a stable medium to incorporate and transport vitamins, with potential applications in foodstuffs. © 2011 Elsevier Ltd.