894 resultados para silica minerals


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This paper reports on the development and validation of a simple and sensitive method that uses solid phase extraction (SPE) and liquid chromatography with ultraviolet detection to analyze fluoxetine (FLX) and norfluoxetine (NFLX) in human plasma samples. A lab-made C18 SPE phase was synthesized by using a sol–gel process employing a low-cost silica precursor. This sorbent was fully characterized by nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM) to check the particles' shape, size and C18 functionalization. The lab-made C18 silica was used in the sample preparation step of human plasma by the SPE-HPLC-UV method. The method was validated in the 15 to 500 ng mL 1 range for both FLX and NFLX using a matrix matched curve. Detection limits of 4.3 and 4.2 ng mL 1 were obtained for FLX and NFLX, respectively. The repeatability and intermediary precision achieved varied from 7.6 to 15.0% and the accuracy ranged from 14.9 to 9.1%. The synthesized C18 sorbent was compared to commercial C18 sorbents. The average recoveries were similar (85–105%), however the lab-made C18 silica showed fewer interfering peaks in the chromatogram. After development and validation, the method using the lab-made C18 SPE was applied to plasma samples of patients under FLX treatment (n ¼ 6). The concentrations of FLX and NFLX found in the samples varied from 46.8–215.5 and 48.0–189.9 ng mL 1 , respectively.

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This study evaluated the effects of organic and inorganic sources of minerals in diets for mid-lactation dairy cows on milk yield and composition, intake and total apparent digestibility of dry matter and nutrients, blood parameters, microbial protein synthesis, and energy and protein balances. Twenty Holstein cows averaging 146.83 +/- 67.34 days in milk and weighing 625.30 +/- 80.37 kg were used. The experimental design was a crossover. Diets were composed of corn silage (50%), ground grain corn, and soybean meal, differing with regard to the sources of trace minerals, plus an organic and inorganic mix. The organic mineral source increased milk fat and fat-corrected milk yield without changing milk yield, intake, or total apparent digestibility. Blood parameters, microbial protein synthesis, and energy and protein balances were not affected by the sources of minerals. Organic sources of minerals improve milk fat yield without affecting other parameters.

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A novel porous silica matrix has been prepared from Pyrex glass, using hydrothermal treatment under saturated-steam condition. This process makes it possible to obtain, in one step, a silica support formed of a homogeneously distributed and interconnected macropore microstructure. The new matrix contains silanol groups that can be used in reactions of surface modification to provide a hybrid material and a selective macrofiltration membrane, and also it can improve chemical inertness. The porous matrix is noncrystalline as obtained and, after thermal treatment at temperatures higher than 950degreesC, exhibits an X-ray pattern characteristic of alpha-cristobalite and low volume contraction. The present samples were characterized by scanning electron microscopy, mercury intrusion porosimetry, nitrogen adsorption-desorption isotherms, infrared spectroscopy, X-ray powder diffractometry, atomic absorption, and high-resolution solid-state nuclear magnetic resonance. The results present a new way of producing a macroporous silica matrix.

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A sample preparation method based on ultrasound assisted-extraction (UAE) of Ca, Mg and P from swine feed has been described. The experiment was performed to cover the variables influencing the sonication process and, the method validation using standard reference material. Final solutions obtained upon sonication were analyzed by flame atomic absorption spectrometry (for Ca and Mg) and by UV-vis spectrophotometry (for P). The best conditions for metal extraction were as follows: sample mass: 100 mg in 20 mL 0.10 mol/L HCl, a particle size: <60 μm, sonication time: 5 cycles of 10 s and ultrasound power: 102 W. The UAE method was applied in digestibility assays in different piglet feeds and their results showed that it is highly comparable (P > 0.05) to the other methods used for such purposes, as block digestion, and offered a Ca, Mg and P method of quantification limit of 10.6, 12.4 and 14 mg/kg, respectively. The major advantages of the UAE method compared to other methods are the high treatment rate, low reagent usage in the extracts and, it does not generate toxic residues that might negatively affect human health and the environment, accompanied by good precision and accuracy.

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Ordered mesoporous, highly luminescent SiO2 particles have been synthesized by spray pyrolysis from solutions containing tetraethylorthosilicate (TEOS), Eu(NO3)3.6H2O, and cetyltrimethylammonium bromide (CTAB) as structure-directing agents. The 1,10-phenantroline (Phen) molecules were coordinated in a post-synthesis step by a simple wet impregnation method. In addition, other matrices were also prepared by the encapsulation of europium complex Eu(fod)3 (where fod = 6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octanedionato) into mesoporous silica, and then the Phen molecules were encapsulated by different impregnation steps, after which the luminescence properties were investigated. The obtained materials were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder x-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Powders with polydisperse spherical grains were obtained, displaying an ordered hexagonal array of mesochannels. Luminescence results revealed that Phen molecules had been successfully coordinated as an additional ligand in the Eu(fod)3 complex into the channels of the mesoporous particles without disrupting the structure.