Novas fases estacionárias à base de sílica para cromatografia líquida de alta eficiência

The present work reviews recent advances in the preparation of new reversed phase packing materials such as sterically protected, bidentate, hybrid organic-inorganic and monolithic phases and phases containing embedded polar groups. The bonding chemistry involved in the preparation of these phases as well as their advantages over conventional C8 and C18 reversed phases are discussed. Understanding the reasons behind the development of these newer column packings helps analysts select the best stationary phase for a given application.

Theoretical investigations of the bulk modulus in the tetra-cubic transition of PbTiO3 material

Resulting from ion displacement in a solid under pressure, piezoelectricity is an electrical polarization that can be observed in perovskite-type electronic ceramics, such as PbTiO3, which present cubic and tetragonal symmetries at different pressures. The transition between these crystalline phases is determined theoretically through the bulk modulus from the relationship between material energy and volume. However, the change in the material molecular structure is responsible for the piezoelectric effect. In this study, density functional theory calculations using the Becke 3-Parameter-Lee-Yang-Parr hybrid functional were employed to investigate the structure and properties associated with the transition state of the tetragonal-cubic phase change in PbTiO3 material.

DESENVOLVIMENTO DE MATERIAIS HÍBRIDOS MICRO-MESOPOROSOS DO TIPO ZSM-12/MCM-41

Micro-mesoporous hybrid materials of ZSM-12/MCM-41 type with different micro- and mesoporosity contributions were prepared by a procedure that uses the desilication of the zeolite in an alkaline medium, followed by recrystallization onto the mesostructure, where the zeolite is used as the silica source in the formation of mesoporous phase. The materials were characterized by X-ray diffraction, nitrogen adsorption-desorption at 77 K, scanning electron microscopy and thermal analysis. The results showed that the methodology utilized is efficient for obtaining hybrid materials of ZSM-12/MCM-41 type with optimized micro-and mesoporosity.

Excretion-secretion products and proteases from live Sporothrix schenckii yeast phase: immunological detection and cleavage of human IgG

Antigenic preparations from Sporothrix schenckii usually involve materials from mixed cultures of yeast and mycelia presenting cross-reactions with other deep mycoses. We have standardized pure yeast phase with high viability of the cells suitable to obtain specific excretion-secretion products without somatic contaminations. These excretion-secretion products were highly immunogenic and did not produce noticeable cross-reactions in either double immunodiffusion or Western blot. The antigenic preparation consists mainly of proteins with molecular weights between 40 and 70 kDa, some of them with proteolytic activity in mild acidic conditions. We also observed cathepsin-like activity at two days of culture and chymotrypsin-like activity at four days of culture consistent with the change in concentration of different secreted proteins. The proteases were able to cleave different subclasses of human IgG suggesting a sequential production of antigens and molecules that could interact and interfere with the immune response of the host.

Ostwald ripening in porous materials

The process of coarsening of an ensemble of clusters is investigated for the case that elastic strains due to matrix - cluster interactions change the process qualitatively as compared with dependencies established theoretically first by Lifshitz and Slezov. Such a qualitatively different behavior occurs always when the energy of elastic deformation in cluster growth increases more rapidly than linear with the volume of a cluster. Analytic solutions, for limiting cases, as well as numerical solutions, for the general case of coarsening in an ensemble of pores with a given pore size distribution, are presented. Possible applications are discussed.

Biologia do saguirú (Characidae, Curimatinae)

In Brazil all the fishes belonging to the sub-family Curimatinae are called « saguirú ». The present work gives a biological study of the Curimatus elegans Steind., a small fish without any economical importance, which is to be found along the whole brazilian coast, down till Paraguay. The specimens utilized for the present study come from Fortaleza (Ceará, north-eastern Brazil). The C. elegans is « ilyophagus », that means, it feeds itself exclusively with those organic materials to be found in mud, specially with microscopical algae. The intestines are very extent, some of them measuring about 9 to 11 times body's length. Studies have been made about growth and age of the C. elegans; the biggest sizes found were of 153 mm. for females and 88 mm. for males. The C. elegans shows developed sexual glands during a long period (April to September). The movements of the spermatozoa, in contact with water is of 40 to 50 seconds of intense movements, ceasing after 70 to 100 seconds. In contact with 0.5% NaCl-solution spermatozoa show a big increase in movements-time, that can last till about 25 minutes. The eggs' diameter measures 0.70 to 0.73 mm., mature and hydrated it attains 0.93 to 1,00 mm. There is a certain correlation between the size of the body and the quantity of eggs. Big specimens can produce a total of 200.000 eggs. The average quantity contained in 1 gr. and 1 cc. is 6018 and 6229 eggs, respectively. Maturity and spawning in laboratory has been obtained due to injections of suspension of fish-hypophysis. Three or four hours after the injection, fishes show more movement and evident signs of excitation, proceeding spawning after 5 to 6 hours. Males, persecuting females, describe successive circles (merry-go-round) - carroussel), swimming side by side with females up to water's surface, where sexual products are start beating dry, for there is no blood yet. Circulation-scheme is to be found on fig. 4 and 5. The swim-bladder and the stomach are but delineated; the intestine is formed by a cylindric tube, all closed. At the place, where later on there will open the mouth, we find a group of ciliary hairs that produce a liquid current, very evident by the semi-circle formed by attached solid particles. After 36 hours, opening of the mouth and formation of the gill slits begin. At the age of 90 hours (4 mm.) the larvas swim well and start to feed themselves; the digestive tube is now all open and the swimbladder works already. During the first days of life, larvas have an adhesive organ situated at their frontal region (fig. 7) in form of a crescent, by means of which they hang to surrounding vegetation (fig. 6). When the larva begins to swim and to feed itself and its yolk are having been absorbed. the adhesive organ retracts and disappears. While larvas and alevins feed themselves with plancton, they have small eye-teeth, which disappear,. when fishes become « ilyophagus ». There exist too, during their life as larvas, pharyngeal-teeth. The lateral line appears in the larva after 16 to 18 days; more or less at the same time all fins are completely developed. Shortly after, first scales appear (20 to 23 days). Evolution of intestines twisting followed (fig. 9). Larvas show at different parts of their bodies small of organs excretory functions, that are constituted by bottons in serial disposition, every one with an excretory canal that opens towards the outside. These formations disappear suddenly when larvas attain their phase of alevin. The existence of a great number of said formations at the caudal fin (fig. 12) is of great interest. In our experiences of breeding we have employed several thousands of C. elegans larvas in different environs and we made conditions of surrounding change (illumination), depth of water, temperature, presence of sand at bottom of aquariums and without sand, food). In this way we could compare the results obtained, estimate the action of each factor for the realisation of a good bring-up of larvas.

When the non-contrast-enhanced phase is unnecessary in abdominal computed tomography scans? A retrospective analysis of 244 cases

Objective: To evaluate the necessity of the non contrast-enhanced phase in abdominal computed tomography scans. Materials and Methods: A retrospective, cross-sectional, observational study was developed, evaluating 244 consecutive abdominal computed tomography scans both with and without contrast injection. Initially, the contrast-enhanced images were analyzed (first analysis). Subsequently, the observers had access to the non-contrast-enhanced images for a second analysis. The primary and secondary diagnoses were established as a function of the clinical indications for each study (such as tumor staging, acute abdomen, investigation for abdominal collection and hepatocellular carcinoma, among others). Finally, the changes in the diagnoses resulting from the addition of the non-contrast-enhanced phase were evaluated. Results: Only one (0.4%; p > 0.999; non-statistically significant) out of the 244 reviewed cases had the diagnosis changed after the reading of non-contrast-enhanced images. As the secondary diagnoses are considered, 35 (14%) cases presented changes after the second analysis, as follows: nephrolithiasis (10%), steatosis (3%), adrenal nodule (0.7%) and cholelithiasis (0.3%). Conclusion: For the clinical indications of tumor staging, acute abdomen, investigation of abdominal collections and hepatocellular carcinoma, the non-contrast-enhanced phase can be excluded from abdominal computed tomography studies with no significant impact on the diagnosis.

Susceptibility weighted imaging: differentiating between calcification and hemosiderin

Objective:To present a detailed explanation on the processing of magnetic susceptibility weighted imaging (SWI), demonstrating the effects of echo time and sensitive mask on the differentiation between calcification and hemosiderin.Materials and Methods:Computed tomography and magnetic resonance (magnitude and phase) images of six patients (age range 41– 54 years; four men) were retrospectively selected. The SWI images processing was performed using the Matlab’s own routine.Results:Four out of the six patients showed calcifications at computed tomography images and their SWI images demonstrated hyperintense signal at the calcification regions. The other patients did not show any calcifications at computed tomography, and SWI revealed the presence of hemosiderin deposits with hypointense signal.Conclusion:The selection of echo time and of the mask may change all the information on SWI images, and compromise the diagnostic reliability. Amongst the possible masks, the authors highlight that the sigmoid mask allows for contrasting calcifications and hemosiderin on a single SWI image.

Solid phase extraction of iron and lead in environmental matrices on amberlite xad-1180/pv

A solid phase extraction procedure using Amberlite XAD-1180/Pyrocatechol violet (PV) chelating resin for the determination of iron and lead ions in various environmental samples was established. The procedure is based on the sorption of lead(II) and iron(III) ions onto the resin at pH 9, followed by elution with 1 mol/L HNO3 and determination by flame atomic absorption spectrometry. The influence of alkaline, earth alkaline and some transition metals, as interferents, are discussed. The recoveries for the spiked analytes were greater than 95%. The detection limits for lead and iron by FAAS were 0.37 µg/L and 0.20 µg/L, respectively. Validation of the method described here was performed by using three certified reference materials (SRM 1515 Apple Leaves, SRM 2711 Montana Soil and NRCC-SLRS-4 Riverine Water). The procedure was successfully applied to natural waters and human hair.

Preconcentration of copper from natural water samples using ligand-less in situ surfactant-based solid phase extraction prior to FAAS determination

In the present work, a simple and rapid ligand-less, in situ, surfactant-based solid phase extraction for the preconcentration of copper in water samples was developed. In this method, a cationic surfactant (n-dodecyltrimethylammonium bromide) was dissolved in an aqueous sample followed by the addition of an appropriate ion-pairing agent (ClO4-). Due to the interaction between the surfactant and ion-pairing agent, solid particles were formed and subsequently used for the adsorption of Cu(OH)2 and CuI. After centrifugation, the sediment was dissolved in 1.0 mL of 1 mol L-1 HNO3 in ethanol and aspirated directly into the flame atomic absorption spectrometer. In order to obtain the optimum conditions, several parameters affecting the performance of the LL-ISS-SPE, including the volumes of DTAB, KClO4, and KI, pH, and potentially interfering ions, were optimized. It was found that KI and phosphate buffer solution (pH = 9) could extract more than 95% of copper ions. The amount of copper ions in the water samples varied from 3.2 to 4.8 ng mL-1, with relative standard deviations of 98.5%-103%. The determination of copper in water samples was linear over a concentration range of 0.5-200.0 ng mL-1. The limit of detection (3Sb/m) was 0.1 ng mL-1 with an enrichment factor of 38.7. The accuracy of the developed method was verified by the determination of copper in two certified reference materials, producing satisfactory results.