Extrações de óleos de sementes de citros e suas atividades sobre a formiga cortadeira Atta sexdens e seu fungo simbionte

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

Método multiresiduo para determinar pesticidas en frutas por extracción con fluido supercrítico

A rapid and reliable method for the determination of 25 compounds selected from four classes of pesticides in samples of fresh apples, grapes, pears, and strawberries purchased at a local supermarket, is presented. The study describes two different methods of extraction: solid-liquid extraction with acetone and supercritical fluid extraction. Clean-up was based on aminopropyl cartridge extraction followed by gas chromatography with an electron capture detector for simultaneous determinations. Confirmatory analysis was carried out by gas chromatography with mass spectrometry in the selected-ion monitoring (SIM) mode. Extraction efficiencies were directly compared and the methods were applied to the analysis of real samples. Recoveries for a majority of pesticides from standard samples at enrichment levels of 0.04-0.10 mg/ kg ranged from 77 to 96 % for both methods. The supercritical fluid extraction method showed good limits of detection (less than 0.01 mg/kg, depending on the pesticide and matrix) as well as minimizing environmental concerns, time, and laboratory effort. © 2006 Centro de Información Tecnológica.

From coffee industry waste materials to skin-friendly products with improved skin fat levels

Spent coffee grounds (SCG), which are the residue obtained from the treatment of coffee with hot water or steam, can be used for industrial applications, due to the high content in lipids. The cosmetic products might be a suitable application for these types of residues because the barrier properties of the stratum corneum (SC) are largely dependent on the intactness of the lipid lamellae that surrounds the corneocytes. The purpose of this work was to assess the feasibility of using the lipid fraction of SCG extracted with supercritical carbon dioxide in the development of new cosmetic formulations with improved skin lipids (sebum) and hydration. The use of spent coffee lipid extract in cosmetic industry seems to be a suitable approach to recycle the wastes from coffee industry. Emulsion containing 10% of the lipid fraction of SCG (SpentCofOil cream) presented promising characteristics in the improvement of sebum skin levels with a good acceptance by consumers when compared to an emulsion containing 10% w/w of green coffee oil (GreenCofOil cream) and a placebo without coffee oil (NoCofOil cream). Practical applications: In this work, the authors develop and characterize a cream containing 10% of the lipid fraction of SCG extracted with supercritical carbon dioxide with improved skin lipids (sebum) and hydration. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Structural characteristics of silica sonogels prepared with different proportions of TEOS and TMOS

Sonohydrolysis of mixtures of tetraethoxysilane (TEOS) and tetramethoxysilane (TMOS) with different TMOS/(TMOS + TEOS) molar ratio R was carried out to obtain similar to 2.0 x 10(-3) mol SiO2/cm(3) and similar to 86%-volume liquid phase wet gels. Aerogels were obtained by supercritical CO2 extraction in autoclave. The samples were analyzed by small-angle X-ray scattering (SAXS) and nitrogen adsorption. The structure of the wet gels can be described as a mass fractal structure with fractal dimension D similar to 2.2 and characteristic length increasing from similar to 4.6 nm for pure TEOS to similar to 6.4 nm for pure TMOS. A fraction of the porosity is eliminated with the supercritical process. The fundamental role of the TMOS/(TMOS + TEOS) molar ratio on the structure of the aerogels is to increase the porosity and the pore mean size as R changes from pure TEOS to pure TMOS. The supercritical process increases the mass fractal dimension and shortens the fractality domain in the mesopore region. A secondary structure appearing in the micropore region of the aerogels can be described as a mass/surface fractal structure with correlated mass fractal dimension D-m similar to 2.6 and surface fractal dimension D-s similar to 2.3. (C) 2007 Elsevier B.V. All rights reserved.

Structural properties of silica gels prepared from oxalic-acid-catalyzed tetraethoxysilane sonohydrolysis

About similar to 2.1 x 10(-3) Mol SiO2 cm(-3) and similar to 88%-volume liquid-phase silica wet gels were prepared from oxalic-acid-catalyzed tetraethoxysilane (TEOS) sonohydrolysis. Aerogels were obtained by supercritical CO2 extraction. The samples were analyzed by thermogravimetry, small-angle X-ray scattering and nitrogen adsorption. Wet gels can be described as mass fractal structures with fractal dimension D similar to 1.94 and structural characteristic length zeta changing between similar to 3.3 to similar to 3.0 nm in the studied range of the catalyst concentration. A fraction of the porosity is apparently eliminated in the supercritical process. The values of the BET specific surface S-BET, the total pore volume V-p and the mean pore size l(p) of the aerogels were found to change almost randomly around the mean values S-BET = 874 m(2) g(-1), V-p = 0.961 cm(3) g(-1) and l(p) = 4.4 nm with catalyst concentration variation. These values were not substantially different from those from an equivalent HCl-catalyzed aerogel. (c) 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Structural characteristics of silica sonogels prepared with additions of isopropyl alcohol

Wet silica gels with similar to 1.4 x 10(-3) mol SiO2/cm(3) and similar to 92 vol% liquid phase were obtained from sonohydrolysis of tetraethoxysilane (TEOS) with different additions of isopropyl alcohol ( IPA). The IPA/TEOS molar ratio R was changed from 0 to 4. Aerogels were obtained by supercritical CO2 extraction. The samples were analyzed by small-angle X-ray scattering (SAXS) and nitrogen adsorption. The wet gels exhibit mass fractal structure with fractal dimension increasing from D similar to 2.10 to D similar to 2.22, characteristic length xi decreasing from similar to 9.5 to similar to 6.9 nm, as R increases from 0 to 4, and an estimated characteristic length for the primary silica particles lower than similar to 0.3 nm. The supercritical process apparently eliminates a fraction of the porosity, increasing the mass fractal dimension and shortening the fractality domain in the mesopore region. The fundamental role of isopropyl alcohol on the structure of the resulting aerogels is to decrease the porosity and the pore mean size as R changes from pure TEOS to R = 4. A secondary structure appearing in the micropore region of the aerogels can be described as a mass/surface fractal structure, with correlated mass fractal dimension D-m similar to 2.7 and surface fractal dimension D-s similar to 2.3, as inferred from SAXS and nitrogen adsorption data.

Preparação de dispersões sólidas de praziquantel com polivinilpirrolidona pelo processo do fluido supercrítico

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Análise estrutural de aerogéis via espalhamento de luz a baixo ângulo

The sol-gel process is a method for obtaining vitreous or vitro-ceramic materials which, are prepared a sol and by drying the liquid phase. This technique has been used extensively for the preparation of glassy gels, films, fibers and particles from the hydrolysis and polycondensation reactions of metal alkoxides. The usual methods for drying are: evaporation drying (xerogels), freeze drying (criogéis) and via supercritical CO2 extraction (aerogels). In the present work, we studied the preparation of silica gels by the sol-gel process from the hydrolysis of alkoxides tetraethylorthosilicate (TEOS) and 3-glycidoxypropyltrimethoxysilane (GPTS). The hydrolysis was promoted from GPTS and TEOS in proportion (4: 1) under acidic conditions. The hydrolysis reaction was promoted inside a Becker at room temperature. After hydrolyses the prepared sol had pH 2, and kept under mechanical agitation for a period of 1 hour. In order to accelerate the polycondensation reaction, the pH was corrected to a value near 5 by slowly adding NH4OH. Then the sols were leaked in sealed polycarbonate containers and maintained for 20 days at 40°C for gelation. Silica aerogels were prepared via supercritical CO2 extraction of the wet gel at temperature and pressure higher than 31°C and 74 atm, in an autoclave specially developed for the process. The structural characteristics were studied in the dry gel (aerogel). Aerogels were then characterized by nitrogen adsorption and small angle light scattering. The nitrogen adsorption data were analyzed for the determination of the BET specific surface (SBET), the total pore volume Vp, the pore mean size (lP=4Vp/SBET), the particle mean size (lS) and the pore size distribution (PSD). And the data from small angle light scattering were analyzed to determine the correlation function (γ'), the area per unit volume (S/V), average pore size (l ) and the average particle size...

Influence of different extraction methods on the yield and linalool content of the extracts of Eugenia uniflora L.

This work has been developed using a sylvestral fruit tree, native to the Brazilian forest, the Eugenia uniflora L., one of the Mirtaceae family. The main goal of the analytical study was focused on extraction methods themselves. The method development pointed to the Clevenger extraction as the best yield in relation to SFE and Soxhlet. The SFE method presented a good yield but showed a big amount of components in the final extract, demonstrating low selectivity. The essential oil extracted was analyzed by GC/FID showing a large range of polarity and boiling point compounds, where linalool, a widely used compound, was identified. Furthermore, an analytical solid phase extraction method was used to clean it up and obtain separated classes of compounds that were fractionated and studied by GC/FlD and GUMS. (c) 2006 Elsevier B.V. All rights reserved.

Lignin from sugar cane bagasse: Extraction, fabrication of nanostructured films, and application

Four lignin samples were extracted from sugar cane bagasse using four different alcohols (methanol, ethanol, n-propanol, and 1-butanol) via the organosolv-CO2 supercritical pulping process. Langmuir films were characterized by surface pressure vs mean molecular area (Pi-A) isotherms to exploit information at the molecular level carrying out stability tests, cycles of compression/expansion (hysteresis), subphase temperature variations, and metallic ions dissolved into the water subphase at different concentrations. Briefly, it was observed that these lignins are relatively stable on the water surface when compared to those obtained via different extraction processes. Besides, the Pi-A isotherms are shifted to smaller molecular areas at higher subphase temperatures and to larger molecular areas when the metallic ions are dissolved into the subphase. The results are related to the formation of stable aggregates (domains) onto the water subphase by these lignins, as shown in the Pi-A isotherms. It was found as well that the most stable lignin monolayer onto the water subphase is that extracted with 1-butanol. Homogeneous Langmuir-Blodgett (LB) films of this lignin could be produced as confirmed by UV-vis absorption spectroscopy and the cumulative transfer parameter. In addition, FTIR analysis showed that this lignin LB film is structured in a way that the phenyl groups are organized preferentially parallel to the substrate surface. Further, these LB films were deposited onto gold interdigitated electrodes and ITO and applied in studies involving the detection of Cd+2 ions in aqueous solutions at low concentration levels throughimpedance spectroscopy and electrochemical measurements. FTIR spectroscopy was carried out before and after soaking the thin films into Cd+2 aqueous solutions, revealing a possible physical interaction between the lignin phenyl groups and the heavy metal ions. The importance of using nanostructured systems is demonstrated as well by comparing both LB and cast films.

Assessing melatonin and its oxidative metabolites amounts in biological fluid and culture medium by liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS)

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