Valdinete Lins da Silva

Nanoencapsulation of quercetin and resveratrol into elastic liposomes.

Based on the fact that quercetin (QUE) and resveratrol (RES) induce a synergic inhibition of the adipogenesis and increase apoptosis in adipocytes, and that sodium deoxycholate (SDC) has necrotic effects, the nanoencapsulation of QUE and RES into SDC-elastic liposomes is proposed as a new approach for dissolving the subcutaneous fat. The concentration of constituents and the effect of the drug incorporation into cyclodextrin inclusion complexes on the stability of QUE/RES-loaded liposomes were studied. The best liposomal formulation reduced the use of phosphatidylcholine and cholesterol in 17.7% and 68.4%, respectively. Liposomes presented a mean diameter of 149nm with a polydispersion index of 0.3. The zeta potential of liposomes was slightly negative (-13.3mV) due to the presence of SDC in the phospholipid bilayer. Encapsulation efficiency of QUE and RES into liposomes was almost 97%. To summarize, QUE/RES-loaded elastic liposomes are stable and suitable for subcutaneous injection, thereby providing a new strategy for reducing subcutaneous fat.

Flow-injection amperometric determination of dopamine in pharmaceuticals using a polyphenol oxidase biosensor obtained from soursop pulp

The amperometric determination of dopamine (Do) in pharmaceuticals formulations by flow injection analysis (FIA) is proposed. An enzymatically modified carbon paste electrode constituted by 25% (w/w) of polyphenol oxidase obtained from Annona muricata L. tissue, 30% (w/w) of graphite, 30% (w/w) of silicone and 15% (w/w) of 7,7,8,8 tetracyanoquinodimethane (TCNQ), was used as flow-through detector. The flow amperometric detection was carried out at a potential of 0.10 V (vs. Ag/AgCl) when an injected sample volume of 250 microl was inserted on a 0.3 M phosphate buffer carrier solution (pH 7.8) flowing at 2.5 ml/min. The developed biosensor showed good stability and reproducibility, enabling up to 500 determinations in 60 days, without considerable loss of enzymatic activity. The FIA system presented a linear response to Do concentrations in the interval from 2 x 10(-2) to 2 x 10(-4) M, with relative standard deviations lower than 1.5%. The kinetic parameter K(M) for the soluble and immobilized enzyme was 1.45 x 10(-2) and 1.91 x 10(-2) M, respectively. In the analyses of different commercially pharmaceutical formulations a relative deviation lower than about 3.4% was obtained.

Potential of a simplified measurement scheme and device structure for a low cost label-free point-of-care capacitive biosensor

A simplified measurement scheme and device structure aiming at developing a low cost, label-free, point-of-care capacitive biosensor were investigated. The detection principle is the increase of low frequency capacitance between two planar Al electrodes observed after antibody-antigen interaction. The electrodes, deposited on oxidized Si wafers, were covered with an antibody layer, with and without using self-assembled thiol monolayer. Immunoglobulin G (IgG) and cardiac troponin T (TnT) were used as analytes to asses this proposal. The device was able to detect successfully TnT levels in the range 0.07 to 6.83ng/mL in human serum from patients with cardiac diseases and in the range 0.01ng/mL to 5ng/mL for TnT in phosphate buffer saline. An equivalent circuit model able to reproduce the general behavior of experimental capacitance versus frequency curves was presented. The investigated features that have potential to reduce costs and simplify measurements were: use of single, low frequency (1kHz) measurement signal, within the range of low cost portable capacitance meters; employment of a lower cost electrode material, aluminum, instead of gold electrodes; and use of simple and miniaturized planar two-electrodes arrangement, thus making a portable system for point-of-care applications.

Phenanthrene and pyrene oxidation in contaminated soils using Fenton's reagent.

Fentons reagent has shown its applicability to oxidizing these biorefractory organic contaminants. The purpose of this contribution was to investigate the influence of operating parameters on the process efficiency for soil highly contaminated by PAHs. Five variables were selected: pH, reaction time, UV irradiation, hydrogen peroxide concentration and Fe (II) amendment. Their effects on the oxidation of (i) phenanthrene and on (ii) phenanthrene and pyrene present in freshly contaminated soil samples were studied through batch reactor experiments following factorial designs. For phenanthrene oxidation run with a soil contaminated at 700 mg kg(-1), one set of variables enabled us to reach a residual concentration lower than 40 mg kg(-1) (Dutch legislation threshold). The most important factor was the reaction time, followed at a certain distance by UV irradiation, Fe (II), H(2)O(2) concentration and pH, this last variable being the least significant. The possibility of operating without pH adjustment is of importance in the treatment at the field scale. This shows the feasibility of photo-Fenton-like oxidation for the treatment of soil highly contaminated with PAH and the relative importance of the process variables.

Potassium permanganate oxidation of phenanthrene and pyrene in contaminated soils.

Potassium permanganate, widely used in water treatment, has shown its applicability to reduce PAH contamination in groundwater and soils. The first stage to design a treatment at the site scale is the feasibility study at the bench scale, generally performed by means of batch experiments. The aim of the present contribution was to investigate the influence of two factors on PAH degradation in spiked soils, following the method of factorial designs. These factors were the weight ratio KMnO(4)/PAH and the reaction time. Three factorial designs were performed and batch experiments were run to study the degradation of phenanthrene and pyrene on soils spiked at different concentrations, between 700 and 2100 mg kg(-1). We showed that treatment with potassium permanganate significantly reduced PAH concentration, but pyrene was more recalcitrant than phenanthrene. Both variables had negative main effects and a positive two-factor interaction effect: increasing the weight ratio or the reaction time enhanced PAH degradation but the reduction produced by the two factors was lower than the sum of the individual contributions. The comparison of these results with results that we published previously under comparable conditions showed that Fentons reagent was more efficient than potassium permanganate.

A flow-batch internal standard procedure for iron determination in hydrated ethanol fuel by flame atomic absorption spectrometry.

A flow-batch manifold coupled to a flame atomic absorption spectrometer was evaluated to assess the iron content by the internal standard method in hydrated ethanol used as fuel in automotive industry. For this assessment official methods require calibration procedures with matrix matching, making it difficult to obtain accurate results for samples adulterated by the addition of water. Nickel was selected as the internal standard since it is usually absent in samples and because it requires similar conditions of atomization. After procedure optimization, which requires about 4.25mL of sample and standard per measurement, it was possible to get linear analytical response for iron concentrations between 0.12 and 1.40mgL(-1) and a detection limit of 0.04mgL(-1). Eighteen samples were collected randomly from fuel stations in Pernambuco (Brazil) and iron concentration was determined using the proposed procedure. Comparison of results obtained (0.20-1.50mgL(-1)) showed a mean standard error of 3.9%, with 3.8% and 2.3% calculated for the mean variation coefficients of the proposed method and the reference procedure, respectively. For adulterated samples (0.12-0.64mgL(-1)), the mean standard error was 4.8% when compared with the standard addition method. These results allowed concluding that the proposed procedure is adequate to accomplish the determination of iron in ethanol fuel in a large scale basis with a sampling rate of about 10h(-1).

Cyclodextrin-based potentiometric sensors for midazolam and diazepam.

In this work the implementation of benzodiazepine ion-selective electrodes for pharmaceutical formulations control is described. The solid-contact electrodes for midazolam and diazepam are based on polymeric membranes incorporating respectively beta-cyclodextrin and (2-hydroxiproyl)-gamma-cyclodextrin as ionophores, 2-fluorophenyl 2-nitrophenyl ether as plasticizer and potassium tetrakis (p-chlorophenyl) borate as ionic additive. For conventionally shaped midazolam electrode a slope of 61.9+/-1.3 mVdec(-1), a LLLR of 5.7+/-2.7 x 10(-4)gL(-1) and pH range of 2.6-5.4 was obtained, while the corresponding values for diazepam electrodes were of 67.6+/-3.0 mVdec(-1), 4.9+/-1.5 x 10(-2)gL(-1) and 1.9-2.7 pH units, respectively. Membrane optimization was based on the molar ratio between the ionophore and additive for midazolam and on inclusion cavity of cyclodextrin for diazepam. The miniaturization of the above-described electrodes gave rise to potentiometric detectors for sequential-injection lab-on-valve system with similar characteristics albeit the useful lifetime shortened from 1 year to approximately 15 days under continuous operation. The optimized flow conditions were achieved for sample injection volumes of 20 microL propelled towards the detection cell at the flow rate of 16 microLs(-1) during 80s. Real sample analysis revealed statistical accuracy and between-days precision comparable to the general used chromatographic-based procedure.

PARTIAL CHARACTERIZATION OF PROTEASES FROM STREPTOMYCES CLAVULIGERUS USING AN INEXPENSIVE MEDIUM

The partial characterization of extracellular proteases from Streptomyces clavuligerus NRRL 3585 and 644 mutant was investigated. The enzyme production was carried out in batch fermentation using soy bean filtrate as nitrogen source. Maximum activity was obtained after 96h of fermentation with an initial pH of 7.0. The enzyme was partially purified by ammonium sulphate precipitation. Enzymes from the two strains retained 37% of their initial activities at pH 8.0 after 2 h incubation at 25oC. Enzyme half-life at pH 8.0 and 60oC was 40.30 and 53.32 min, respectively for both strains (partially purified extract). The optimum pH was obtained at pH 7.0-8.0 and 8.4 for enzymes produced for 3585 and 644 strains (crude extract), respectively, and 8.4 and 8.0 for enzymes from the partially purified extract 3585 and 644 strains, respectively. The optimum temperature for the crude extract was 21oC for both strains. However, for the partially preparation the optimum temperature was 50oC and 40°C for S. clavuligerus NRRL 3585 and 644 strains respectively.

Avaliação do processo adsortivo utilizando mesocarpo de coco verde para remoção do corante cinza reativo BF-2R

was used to evaluate the influence of the variables adsorbent mass, particle size and stirring speed on the adsorptive process. Kinetic and adsorption equilibrium studies were performed. Results showed that the kinetic equilibrium was reached after 150 min. Using the Langmuir model, a qmax of 21.9 mg g-1 and k of 0.30 L g-1 was obtained. The mesocarp of coconut, a residue of agribusiness, proved to be an effective alternative technique for the removal of dye in this study.

Adsorption of azo dyes using peanut hull and orange peel: a comparative study

This work proposes the use of agro-industrial wastes, specifically peanut hull (HP) and orange peel (OP), as adsorbents for dyes, such as Remazol Golden Yellow RNL-150% (RYG), Gray Reactive BF-2R (RG) and Reactive Turquoise Q-G125 (RT). Characterization by Brunauer-Emmett-Teller indicates that the adsorbents are mesoporous, with pHzpc values of 5.0 for HP and 4.0 for OP. Fourier transform-infrared spectroscopy identified carbonyl and sulphonic groups. The initial pH of the best-adsorbing solution of the three colours was 2.0. Increasing the concentration of the adsorbent promoted an increase in the percentage of removal until saturation of the adsorbent. In a factorial design, the largest value of q was obtained with 0.25 g of the adsorbent, with a particle size of<0.4 mm and a stirring speed of 300 rpm. Such conditions were used in kinetic studies and studies of adsorption equilibrium. The evolution kinetics were rapid in the first few minutes, and after 180 min the system reached equilibrium. The kinetic model that best fit the experimental data to a 95% confidence level for the F test was the pseudo-second-order model for RYG/HP, RG/OP and RT/OP. There was no significant difference between the kinetic models as evaluated by the F test for RYG/OP, RG/HP and RT/HP. The experimental results indicated favourable dye adsorption characteristics for the adsorbents studied. The results of the F test showed that for RYG and RG, there was no significant difference between the two evaluated models. This study suggests that HP and OP are viable alternatives for the treatment of effluents containing RYG, RG and RT dyes.