Loading of praziquantel in the crystal lattice of solid lipid nanoparticles Studies by DSC and SAXS

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Equilibrium, Thermoanalytical and Spectroscopic Studies to Characterize Phytic Acid Complexes with Mn(II) and Co(II)

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

The role of matrix effects on the quantification of abscisic acid and its metabolites in the leaves of Bauhinia variegata L. using liquid chromatography combined with tandem mass spectrometry

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Laboratory essays on solid residues from an area of sand mining activities at Analandia, São Paulo, Brazil, and implications to the water resources quality

This investigation reports the results of tests performed in a laboratory with solid waste samples from an area belonging to Sibelco Mineracao Ltd., which is located around Analandia municipality, nearly in the center of São Paulo State, Brazil. Dissolution and leaching essays were realized under different experimental conditions in four samples collected from the mining front and decantation pool, with the aim of evaluating the possibility of release of several constituents to the liquid phase.

Determination of herbicides and a metabolite in human urine by liquid chromatography-electrospray ionization mass spectrometry

A method was developed to determine simazine, atrazine and their metabolite, 2-chloro-4,6-diamino-1,3,5-triazine, in urine. The presence of these herbicides in urine may reflect possible exposure to pesticides. Sample preparation involved protein precipitation and solid-phase extraction. The samples were analyzed by high-performance liquid chromatography-mass spectrometry. The detection limits were 0.4 mug/l and the analytes have a linear response in the interval 6-800 mug/l. The precision of the method was reflected in the RSD of <2.4% for the herbicides studied. Based on the detectable herbicide levels from spiked urine samples collected from unexposed volunteers, this method can be used to determine the low levels necessary for establishing reference values of the selected herbicides and the metabolite. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Electrical properties of YSZ/NiO composites prepared by a liquid mixture technique

We report the preparation and characterization of yttria-stabilized zirconia/nickel oxide composites (YSZ/NiO). This composite is the precursor material of the cermet YSZ/Ni, which is used as solid oxide fuel cell anode material. The performance of the anode is strongly dependent on the microstructural properties of the cermet. Therefore, the control of the microstructure of the YSZ/NiO composite is a key step for the fabrication of high-performance anodes. In this study, the composites were prepared by a modified liquid mixture technique. Scanning electron microscopy analysis evidenced the good dispersion of the phases and that NiO nanoparticles are spread over the YSZ surface. Sintered pellets were studied by X-ray diffraction and impedance spectroscopy. The main results show that the composite is comprised of a well-dispersed mixture of the two phases. The electrical conductivity data show that there is a strong dependence of the transport mechanism on the relative composition of phases. (c) 2005 Elsevier Ltd. All rights reserved.

Structural evolution up to 1100 degrees C of xerogels prepared from TEOS sonohydrolysis and liquid phase exchanged by acetone

Silica xerogels were prepared from sonohydrolysis of tetraethoxysilane and exchange of the liquid phase of the wet gel by acetone. Monolithic xerogels were obtained by slow evaporation of acetone. The structural characteristics of the xerogels were studied as a function of temperature up to 1100 degrees C by means of bulk and skeletal density measurements, linear shrinkage measurements and thermal analyses (DTA, TG and DL). The results were correlated with the evolution in the UV-Vis absorption. Particularly, the initial pore structure of the dried acetone-exchanged xerogel was studied by small-angle X-ray scattering and nitrogen adsorption. The acetone-exchanged xerogels exhibit greater porosity in the mesopore region presenting greater mean pore size (similar to 4 nm) when compared to non-exchanged xerogels. The porosity of the xerogels is practically stable in the temperature range between 200 degrees C and 800 degrees C. Evolution in the structure of the solid particles (silica network) is the predominant process upon heating up to about 400 degrees C and pore elimination is the predominant process above 900 degrees C. At 1000 degrees C the xerogels are still monolithic and retain about 5 vol.% pores. The xerogels exhibited foaming phenomenon after hold for 10 h at 1100 degrees C. This temperature is even higher than that found for foaming of non-exchanged xerogels. (c) 2005 Elsevier B.V. All rights reserved.

Determination of aldicarb, aldicarb sulfoxide and aldicarb sulfone in some fruits and vegetables using high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry

An analytical method for the determination of aldicarb, and its two major metabolites, aldicarb sulfoxide and aldicarb sulfone in fruits and vegetables is described. Briefly the method consisted of the use of a methanolic extraction, liquid-liquid extraction followed by solid-phase extraction clean-up. Afterwards, the final extract is analyzed by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry (LC-APCI-MS). The specific fragment ion corresponding to [M-74](+) and the protonated molecular [M+K](+) ion were used for the unequivocal determination of aldicarb and its two major metabolites. The analytical performance of the proposed method and the results achieved were compared with those obtained using the common analytical method involving LC with post-column fluorescence detection (FL). The limits of detection varied between 0.2 and 1.3 ng but under LC-FL were slightly lower than when using LC-APCI-MS. However both methods permitted one to achieve the desired sensitivity for analyzing aldicarb and its metabolites in vegetables. The method developed in this work was applied to the trace determination of aldicarb and its metabolites in crop and orange extracts. (C) 2000 Elsevier B.V. B.V. All rights reserved.

Multiresidue analysis of pesticides in water from rice cultures by on-line solid phase extraction followed by LC-DAD

An automated on-line solid phase extraction procedure followed by liquid chromatography with diode array detection was investigated for the determination of different classes of pesticides in water samples containing varied amount of humic substances. The different pesticides used were: carbendazin, carbofuran, atrazine, diuron, propanil, molinate, alachlor, parathion-ethyl, diazinon, trifluralin and the degradation products deisopropylatrazine and deethylatrazine. Humic substances extracted from a Brazilian sediment were used from 5 to 80 mg/l and their influence on recoveries was evaluated in neutral and acidic media. Recoveries higher than 70% were obtained for all the pesticides, from the preconcentration of 75 mi of aqueous sample fortified at 2 ng/ml using precolumns packed with PLRP-S. Good recoveries were obtained at neutral pH for most of the analytes up to 40 mg/l of humic acid. Only at 80 mg/l the recoveries were significantly affected, both at acidic and neutral pH. The method was applied to the determination of pesticides in river water spiked at 0.1 to 1 ng/ml. Detection limits obtained for water containing 10 mg/l of humic acid were between 0.05 and 0.3 ng/ml.

Determination of the geometrical diarylpropenamine isomers in feces by high-performance liquid chromatography

Diarylpropenamine derivatives are a class of compounds which have been evaluated as potential drug candidates. Here a specific and reproducible HPLC method for the determination of cis- and trans-isomers of the unsubstituted derivative, 3-(4'-bromo-[1,1'-biphenyl]-4-yl)-3-(4-X-phenyl-N,N-dimethyl-2-propen-1-amine (I, where X=H) in feces is described. The analyte I and internal standard, nitro derivative (II, where X=NO2), were isolated from the basified biological matrix using a liquid-liquid extraction with ethyl acetate followed by a solid-phase procedure performed on a silica cartridge. The organic phase was evaporated to dryness, the residue was reconstituted in mobile phase and injected into the HPLC system. The analytes were eluted with ethyl acetate-hexane-triethylamine (59:40:1) in HPLC column (silica) and detected by UV spectrophotometry at 272 nm. Linearity, precision and accuracy data for feces standards after extraction were acceptable. The method has been applied to analyses of feces samples from rats dosed with I, in which it could be anticipated that fecal excretion is quantitatively the major route for I elimination. Copyright (C) 1999 Elsevier Science B.V.

In vitro propagation of Maytenus ilicifolia (Celastraceae) as potential source for antitumoral and antioxidant quinomethide triterpenes production. A rapid quantitative method for their analysis by reverse-phase high-performance liquid chromatography

Cell culture of Maytenus ilicifolia were established in order to produce and to quantify the antitumoral and antioxidant quinonemethide triterpenes. In vitro calli were induced from leaf explants of native plants and cultured in semi-solid medium under controlled conditions of humidity, temperature and photoperiod. The quinonemethide triterpenes showed maximum accumulation in the logarithmic phase growth of the cell culture. A rapid, sensitive and reliable reverse-phase HPLC method was used for quantitative determination of the antitumoral and antioxidant quinonemethide triterpenes, 22β-hydroxymaytenin and maytenin in callus of Maytenus ilicifolia. Well resolved peaks with good detection response and linearity in the range 1.0 - 100 μg/mL were obtained. This quantitative work was performed by an external standard method.

Microstructural and electrical properties of the sofc anode precursor YSZ/NiO composite prepared by A liquid mixture technique

A detailed study of the microstructural and electrical properties of the yttria-stabilized zirconia/nickel oxide (YSZ/NiO) composite was performed. This material is the precursor to the solid oxide fuel cell anode cermet YSZ/Ni. A liquid mixture technique was developed to produce the YSZ/NiO composite to fabricate high-performance SOFC anodes. This technique resulted in fine and homogeneous powders and specimens with high electrical conductivity. The combined results showed that this technique is suitable for the production of the anode cermet.

Non-conventional applications of computerized tomography: Analysis of solid dosage forms produced by pharmaceutical industry

X-ray computed tomography (CT) refers to the cross-sectional imaging of an object measuring the transmitted radiation at different directions. In this work, we describe a non-conventional application of computerized tomography: visualization and improvements in the understanding of some internal structural features of solid dosage forms. A micro-CT X-ray scanner, with a minimum resolution of 30 μm was used to characterize some pharmaceutical tablets, granules, controlled-release osmotic tablet and liquid-filled soft-gelatin capsules. The analysis presented in this work are essentially qualitative, but quantitative parameters, such as porosity, density distribution, tablets dimensions, etc. could also be obtained using the related CT techniques. © 2010 American Institute of Physics.

Thermal tunability of photonic bandgaps in photonic crystal fibers selectively filled with nematic liquid crystal

We address the bandgap effect and the thermo-optical response of high-index liquid crystal (LC) infiltrated in photonic crystal fibers (PCF) and in hybrid photonic crystal fibers (HPCF). The PCF and HPCF consist of solid-core microstructured optical fibers with hexagonal lattice of air-holes or holes filled with LC. The HPCF is built from the PCF design by changing its cladding microstructure only in a horizontal central line by including large holes filled with high-index material. The HPCF supports propagating optical modes by two physical effects: the modified total internal reflection (mTIR) and the photonic bandgap (PBG). Nevertheless conventional PCF propagates light by the mTIR effect if holes are filled with low refractive index material or by the bandgap effect if the microstructure of holes is filled with high refractive-index material. The presence of a line of holes with high-index LC determines that low-loss optical propagation only occurs on the bandgap condition. The considered nematic liquid crystal E7 is an anisotropic uniaxial media with large thermo-optic coefficient; consequently temperature changes cause remarkable shifts in the transmission spectrums allowing thermal tunability of the bandgaps. Photonic bandgap guidance and thermally induced changes in the transmission spectrum were numerically investigated by using a computational program based on the beam propagation method. © 2010 SPIE.

Production of pectate lyase by penicillium viridicatum RFC3 in solid-state and submerged fermentation

Pectate lyase (PL) was produced by the filamentous fungus Penicillium viridicatum RFC3 in solid-state cultures of a mixture of orange bagasse and wheat bran (1 : 1 w/w), or orange bagasse, wheat bran and sugarcane bagasse (1 : 1 : 0.5 w/w), and in a submerged liquid culture with orange bagasse and wheat bran (3%) as the carbon source. PL production was highest (1,500U mL -1 or 300Ug -1 of substrate) in solid-state fermentation (SSF) on wheat bran and orange bagasse at 96 hours. PL production in submerged fermentation (SmF) was influenced by the initial pH of the medium. With the initial pH adjusted to 4.5, 5.0, and 5.5, the peak activity was observed after 72, 48, and 24 hours of fermentation, respectively, when the pH of the medium reached the value 5.0. PL from SSF and SmF were loaded on Sephadex-G75 columns and six activity peaks were obtained from crude enzyme fromSSF and designated PL I, II, III, IV, V, andVI, while five peaks were obtained fromcrude enzyme fromSmF and labeled PL I', II', III', IV', and VII'. Crude enzyme and fraction III from each fermentative process were tested further. The optimum pH for crude PL from either process was 5.5, while that for PL III was 8.0. The maximum activity of enzymes from SSF was observed at 35°C, but crude enzyme was more thermotolerant than PL III, maintaining its maximum activity up to 45°C. Crude enzyme from SmF and PL III' showed thermophilic profiles of activity, with maximum activity at 60 and 55°C, respectively. In the absence of substrate, the crude enzyme from SSF was stable over the pH range 3.0-10.0 and PL III was most stable in the pH range 4.0-7.0. Crude enzyme from SmF retained 70%-80% of its maximum activity in the acid-neutral pH range (4.0-7.0), but PIII showed high stability at alkaline pH (7.5-9.5). PL from SSF was more thermolabile than that from SmF. The latter maintained 60% of its initial activity after 1 h at 55°C. The differing behavior of the enzymes with respect to pH and temperature suggests that they are different isozymes. Copyright © 2010 Viviani Ferreira et al.