Extraction and quantification of phenolic acids and flavonols from Eugenia pyriformis using different solvents

The recovery of phenolic compounds of Eugenia pyriformis using different solvents was investigated in this study. The compounds were identified and quantified by reverse-phase high-performance liquid chromatography coupled with ultraviolet-visible diode-array detector (RP-HPLC-DAD/UV-vis). Absolute methanol was the most effective extraction agent of phenolic acids and flavonols (588.31 mg/Kg) from Eugenia pyriformis, although similar results (p ≤ 0.05) were observed using methanol/water (1:1 ratio). Our results clearly showed that higher contents of phenolic compounds were not obtained either with the most or the least polar solvents used. Several phenolic compounds were identified in the samples whereas gallic acid and quercetin were the major compounds recovered. © 2012 Association of Food Scientists & Technologists (India).

Conductive nanocomposites based on cellulose nanofibrils coated with polyaniline-DBSA via in situ polymerization

Cellulose nanofibrils (CNF) were extracted by acid hydrolysis from cotton microfibrils and nanocomposites with polyaniline doped with dodecyl benzenesulphonic acid (PANI-DBSA) were obtained by in situ polymerization of aniline onto CNF. The ratios between DBSA to aniline and aniline to oxidant were varied in situ and the nanocomposites characterized by four probe DC electrical conductivity, ultraviolet-visible-near infrared (UV-Vis - NIR) and Fourier-transform infrared (FTIR) spectroscopies and X-ray diffraction (XRD). FTIR and UV-Vis/NIR characterization confirmed the polymerization of PANI onto CNF surfaces. Electrical conductivity of about 10 -1 S/cm was achieved for the composites; conductivity was mostly independent of DBSA/aniline (between 2 and 4) and aniline/oxidant (between 1 and 5) molar ratios. X-ray patterns of the samples showed crystalline peaks characteristic of cellulose I for CNF samples, and a mixture of both characteristic peaks of PANI and CNF for the nanocomposites. Field emission scanning electron microscopy (FESEM) characterization corroborated the abovementioned results showing that PANI coated the surface of the nanofibrils. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Voltammetric determination of sulfite using graphite paste electrode modified with nanoparticles of copper pentacyanonitrosylferrate

Copper Pentacyanonitrosylferrate (NCuNP) nanoparticles were prepared in formamide solvent. The material was characterized by Infrared (FTIR), X-Ray Diffraction (XRD) and Ultraviolet-Visible (UV-Vis) Spectroscopy. The Cyclic Voltammogram (CV) the modified graphite paste electrode with NCuNP exhibits two redox couples with (Eθ,)1 = 0.29 and (E θ,)2 = 0.86 V attribute at Cu(I)/Cu (II) and Fe(II)(CN)5NO/Fe(III)(CN) 5NO processes, respectively (KCl = 1.0 mol L-1; v = 20 mV s-1). The redox couple with (Eθ,)2 presents an electrocatalytic response for sulfite. The modified graphite paste electrode gives a linear response of 7.0 × 10-4 to 3.0 × 10-2 mol L-1 (r = 0.998), for sulfite determination with Detection Limit (DL) of 1.76 × 10-3 mol L-1 and an amperometric sensitivity of 3.38 mA/mol L-1 and relative standard desviations ± 3% (n=3). ©The Electrochemical Society.

Acid dye biodegradation using saccharomyces cerevisiae immobilized with polyethyleneimine-treated sugarcane bagasse

Chemical reagents used by the textile industry are very diverse in their composition, ranging from inorganic compounds to polymeric compounds. Strong color is the most notable characteristic of textile effluents, and a large number of processes have been employed for color removal. In recent years, attention has been directed toward various natural solid materials that are able to remove pollutants from contaminated water at low cost, such as sugarcane bagasse. Cell immobilization has emerged as an alternative that offers many advantages in the biodegradation process, including the reuse of immobilized cells and high mechanical strength, which enables metabolic processes to occur under adverse conditions of pH, sterility, and agitation. Support treatment also increases the number of charges on the surface, thereby facilitating cell immobilization processes through adsorption and ionic bonds. Polyethyleneimine (PEI) is a polycationic compound known to have a positive effect on enzyme activity and stability. The aim of the present study was to investigate a low-cost alternative for the biodegradation and bioremediation of textile dyes, analyzing Saccharomyces cerevisiae immobilization in activated bagasse for the promotion of Acid Black 48 dye biodegradation in an aqueous solution. A 1 % concentration of a S. cerevisiae suspension was evaluated to determine cell immobilization rates. Once immobilization was established, biodegradation assays with free and immobilized yeast in PEI-treated sugarcane bagasse were evaluated for 240 h using UV-vis spectrophotometry. The analysis revealed significant relative absorbance values, indicating the occurrence of biodegradation in both treatments. Therefore, S. cerevisiae immobilized in sugarcane bagasse is very attractive for use in biodegradation processes for the treatment of textile effluents. © 2012 Springer Science+Business Media Dordrecht.

Low-temperature synthesis of nanosized bismuth ferrite by the soft chemical method

This paper describes research on a simple low-temperature synthesis route to prepare bismuth ferrite nanopowders by the polymeric precursor method using bismuth and iron nitrates. BiFeO 3 (BFO) nanopowders were characterized by means of X-ray diffraction analyses, (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy (Raman), thermogravimnetric analyses (TG-DTA), ultra-violet/vis (UV/Vis) and field emission scanning electron microscopy (FE-SEM). XRD patterns confirmed that a pure perovskite BiFeO 3 structure with a rhombohedral distorted perovskite structure was obtained by heating at 850 °C for 4 hours. Typical FT-IR spectra for BFO powders revealed the formation of a perovskite structure at high temperatures due to a metal-oxygen bond while Raman modes indicated oxygen octahedral tilts induced by structural distortion. A homogeneous size distribution of BFO powders obtained at 850 °C for 4 hours was verified by FE-SEM analyses. © 2012 Elsevier Ltd and Techna Group S.r.l.

Characterization, and crystal structure of thiophenyl-2-methylidene-2- aminophenol

The Schiff base thiophenyl-2-methylidene-2-aminophenol (ImineOH) is obtained from a stoichiometric mixture of 2-thiophenecarboxaldehyde and 2-aminophenol in ethanol under reflux at 90 C. Its crystal structure is determined by single crystal X-ray diffraction. ImineOH packs in an orthorhombic unit cell in the Pbca space group with the unit cell parameters a = 16.942(4) Å, b = 13.4395(11) Å, and c = 17.5857(12) Å, V = 4004.1(10) Å3, Z = 16. Strong hydrogen bonds are present in the ImineOH structure. Apart from the X-ray study, ImineOH was characterized by elemental analysis (CHN-S) and FT-IR (4000 cm-1 to 400 cm-1), UV-Vis and 13C, 1H, and 15N NMR spectroscopic measurements. © 2013 Pleiades Publishing, Ltd.

Quantification of water in ethanol using a photothermal transparent transducer

Ethanol with added water may be found during the process of assessing its physical and chemical properties. This addition can damage automotive vehicle engines and also may contribute to tax evasion. The present contribution describes a method based on a photothermal transparent transducer to determine the water content in ethanol. A chamber with a window of lithium tantalate coated with a thin layer of indium tin oxide was used, and a 1450-nm laser diode was employed as the excitation source. The results indicated a nearly linear response of the apparatus, as a function of the water content in water/ethanol solutions ranging from 0 to 100 (vol.%). The results for the dependency of the photothermal signal on the laser power and chopping frequency suggested that reliable results can be obtained using laser power and chopping rates above 100 mW and 10 Hz, respectively. The results reported here may be useful in the development of an alternative method that can provide real-time data on the water concentration in ethanol in a rapid, portable and unambiguous way, and that can be easily used in laboratory analyses or in gas stations. © 2013 Elsevier B.V.

Evaluation of the interactions of DNA with the textile dyes Disperse Orange 1 and Disperse Red 1 and their electrolysis products using an electrochemical biosensor

A disposable pencil graphite electrode modified with dsDNA was used in combination with square wave voltammetry in order to evaluate the interaction of DNA with the textile dyes Disperse Orange 1 (DO1) and Disperse Red 1 (DR1), and with the products of their electrolysis. Significant changes in the characteristic oxidation peaks of the guanine and adenine moieties of immobilized dsDNA were observed after incubation of the modified electrode for 180 s in solutions of the dyes in their original forms. The same was observed using the electrolysis products obtained by oxidation and reduction conversions. The oxidation peak currents of the guanine and adenine moieties decreased when the concentrations of DO1 and DR1 were increased up to 5.0 × 10 -6 and 1.0 × 10-6 mol L-1, respectively; the signal decreases were more pronounced after interaction with the oxidized dyes, compared to the reduced compounds. The interactions between DNA and DO1, DR1, and the electrolyzed dyes were further investigated by UV-vis spectrophotometry in solution, and different effects such as hypochromism and hyperchromism were observed in the resulting DNA spectra. The investigated interactions showed clear evidence of changes in the DNA structure, and suggested a predominant intercalation mode leading to damage in the biomolecule. © 2013 Elsevier B.V.

Sulfonation and anticoagulant activity of fungal exocellular β-(1→6)-d-glucan (lasiodiplodan)

An exocellular β-(1→6)-d-glucan (lasiodiplodan) produced by a strain of Lasiodiplodia theobromae (MMLR) grown on sucrose was derivatized by sulfonation to promote anticoagulant activity. The structural features of the sulfonated β-(1→6)-d-glucan were investigated by UV-vis, FT-IR and 13C NMR spectroscopy, and the anticoagulant activity was investigated by the classical coagulation assays APTT, PT and TT using heparin as standard. The content of sulfur and degree of substitution of the sulfonated glucan was 11.73% and 0.95, respectively. UV spectroscopy showed a band at 261 nm due to the unsaturated bond formed in the sulfonation reaction. Results of FT-IR and 13C NMR indicated that sulfonyl groups were inserted on the polysaccharide. The sulfonated β-(1→6)-d-glucan presented anticoagulant activity as demonstrated by the increase in dose dependence of APTT and TT, and these actions most likely occurred because of the inserted sulfonate groups on the polysaccharide. The lasiodiplodan did not inhibit the coagulation tests. © 2012 Elsevier Ltd.

Pharmacokinetic Profile of A New Diclofenac Prodrug without Gastroulcerogenic Effect

Gastrotoxicity is a major problem for long-term therapy with non-steroidal anti-inflammatory drugs (NSAIDs). DICCIC (1-(2,6-dichlorophenyl)indolin-2-one) is a new diclofenac prodrug, which has proven anti-inflammatory activity without gastroulcerogenic effect. The aim of this work was to compare the pharmacokinetic profiles of diclofenac from DICCIC (7.6 mg/kg equivalent to 8.1 mg/kg diclofenac) and diclofenac (8.1 mg/kg) administration in Wistar rats weighing 250-300 g (n=20). The doses were calculated by interspecific allometric scaling based on the 2 mg/kg from diary human dose of diclofenac. Blood samples were collected in heparinized tubes via the femoral artery through the implanted catheter. The plasma was separated and quantitation was made in a HPLC system with a UV-Vis detector. The confidence limits of the bioanalytical method were appropriate for its application in a preclinical pharmacokinetic study. The AUC of diclofenac from DICCIC (53.7± 5.8 ug/mL.min) was significantly less (Mann Whitney test, p<0.05) than that of diclofenac from diclofenac administration (885.9 ± 124,8 ug/mL.min). Terminal half-life of diclofenac from DICCIC (50.1 ± 17.2 min) was significantly less (Mann Whitney test, p<0.05) than that of diclofenac from diclofenac administration (247.4 ± 100.9 min). Still the parameters clearance and distribution volume were calculated for diclofenac from diclofenac, whose results were 9.2 ±1.2 mL/min.kg and 3.3 ±1.2 L/kg, respectively. The results of DICCIC from DICCIC administration were 108.9 ± 19.6 mL/min.kg and 7.8 ± 2.4 L/kg for clearance and distribution volume, respectively. The pharmacokinetic profile demonstrated that there was an increase in diclofenac elimination and a lower exposure to diclofenac with administration of DICCIC compared to diclofenac. © 2013 Bentham Science Publishers.

New ruthenium(II)/phosphines/diimines complexes: Promising antitumor (human breast cancer) and Mycobacterium tuberculosis fighting agents

The synthesis and characterization of ruthenium compounds of the type [RuCl2(P)2(N-N)] [(P)2 = (PPh3) 2, dppb = 1,4-bis(diphenylphosphino)butano; dppp = 1,3-bis(diphenylphosphino)propane; N-N = 5,5′-dimethyl-2,2′dipyridyl (5,5′-mebipy) or 4,4′-dimethyl-2,2′dipyridyl (4,4′-mebipy)] are described. The complexes were characterized using elemental analysis, UV-Vis and infrared spectroscopies, cyclic voltammetry, and X-ray crystallography. In vitro evaluation of the complexes, using the MTT methodology, revealed their cytotoxic activities in a range of 5.4-15.7 μM against the MDA-MB-231 breast tumor cells and showed that, in this case, they are more active than the reference metallodrug cisplatin. The in vitro antimycobacterial activities of the complexes had their Minimum Inhibitory Concentration (MIC) for MTB cell growth measured, by the REMA method. The MICs for these complexes were found to be between 12.5 and 25.0 μg/mL. The results are comparable with the second line drug cycloserine (MIC = 12.5-50.0 μg/mL), commonly used in the treatment of TB. © 2013 Elsevier Ltd. All rights reserved.

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.

Validation of an alternative analytical method for the quantification of antioxidant activity in plant extracts

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Electrochemical Properties of Oxo-Manganese Complex Biomimicking Enzyme Active Sites and Its Electrocatalytic Application for Dopamine Determination

This work describes the characterization of the [Mn2 IV,IVO2(terpy)2(H2O)2]4+ complex in aqueous solution by UV-vis spectrophotometry, cyclic voltammetry, and linear sweep voltammetry with a rotating disk electrode. The pH effect, potential scan rate, effect of perfluorosulfonate polymer, and anion of supporting electrode on the electrochemical behavior of the modified electrode for better performance were investigated. The potential peak of the modified electrode was linearly dependent upon the ratio [ionic charge]/[ionic radius]. The modified electrode exerted an electrocatalytic effect on dopamine oxidation in aqueous solution with a decrease in the overpotential compared with the unmodified glassy carbon electrode. This way, the modified electrode showed an enzymatic biomimicking behavior. Tafel plot analyses were used to elucidate the kinetics and mechanism of dopamine oxidation. © 2013 Springer Science+Business Media New York.

Optically transparent membrane based on bacterial cellulose/ polycaprolactone

Optically transparent membranes from bacterial cellulose (BC)/polycaprolactone (PCL) have been prepared by impregnation of PCL acetone solution into dried BC membranes. UV-Vis measurements showed an increase on transparency in BC/PCL membrane when compared with pristine BC. The good transparency of the BC/PCL can be related to the presence of BC nanofibers associated with deposit of PCL nano-sized spherulites which are smaller than the wavelength of visible light and practically free of light scattering. XRD results show that cellulose type I structure is preserved inside the BC/PCL membrane, while the mechanical properties suggested indicated that PCL acts as a plasticizer for the BC membrane. The novel BC/PCL membrane could be used for preparation of fully biocompatible flexible display and biodegradable food packaging.