Crystallization of progesterone polymorphs using polymer-induced heteronucleation (PIHn) method

Progesterone is a natural hormone steroid used in humans for several treatments and in livestock for artificial insemination, which exhibits two polymorphic forms at ambient conditions: form 1 and form 2. Form 2 is metastable and more soluble than form 1; however, it is not suitable to use as powder raw material because it transforms into form 1 by the effects of grinding. A polymorphic screening of progesterone based on polymer-induced heteronucleation method was performed as an alternative to prepare the metastable form. Polyvinyl alcohol, hydroxypropyl methylcellulose (HPMC), dextran, gelatin, polyisoprene (PI) and acrylonitrile-butadiene (NBR) copolymer were used. Crystals were prepared from 0.5, 10 and 40?mg/mL solutions in acetone at room temperature by solvent evaporation. The samples were characterized by X-ray powder diffraction, differential scanning calorimetry (DSC), scanning electron microcopy and attenuated total reflectance infrared Fourier transform spectroscopy. Form 1 was nucleated from 40?mg/mL solutions on the six polymers and from 10?mg/mL solutions on PI and NBR. The mixture of form 1 and form 2 was obtained from 10?mg/mL solution on HPMC, dextran and gelatin and from 0.5?mg/mL solution crystallizations. Therefore, the polymeric devices, which crystallized the metastable and more soluble polymorph (2) of progesterone, would be a promissory alternative for the pharmaceutical applications.     

A New Hand-Held Microsystem Architecture for Biological Analysis

This paper presents a hand-held microsystem based on new fully integrated magnetoresistive biochips for biomolecular recognition (DNA hybridization, antibody antigen interaction, etc.). Magnetoresistive chip surfaces are chemically treated, enabling the immobilization of probe biomolecules such as DNA or antibodies. Fluid handling is also integrated in the biochip. The proposed microsystem not only integrates the biochip, which is an array of 16times16 magnetoresistive sensors, but it also provides all the electronic circuitry for addressing and reading out each transducer. The proposed architecture and circuits were specifically designed for achieving a compact, programmable and portable microsystem. The microsystem also integrates a hand-held analyzer connected through a wireless channel. A prototype of the system was already developed and detection of magnetic nanoparticles was obtained. This indicates that the system may be used for magnetic label based bioassays     

Probing the thermal decomposition process of layered double hydroxides through in situ <Superscript>57</Superscript>Fe Mössbauer and in situ X-ray diffraction experiments

The thermal decomposition properties of Mg–Fe hydrotalcites were studied through in situ ⁵⁷Fe Mössbauer spectroscopy and in situ X-ray diffraction. Abrupt changes in the quadrupolar splitting measured in the Mössbauer spectra revealed a phase transition from the starting lamellar structure to a new crystalline arrangement. By analyzing the Mössbauer parameters we show that the material is highly disordered in the 300–400 °C temperature range. This hypothesis is confirmed by the X-ray results whose diffractograms indicated the collapse of the lamellar structure and the formation of a solid solution.     

On the stabilizing behavior of zirconia: A Combined experimental and theoretical study

Reactive zirconia powder was synthesized by the complexation of zirconium metal from zirconium hydroxide using a solution of 8-hydroxiquinoline. The kinetics of zirconia crystallization was followed by X-ray diffraction, scanning electron microscopy and surface area measured by the nitrogen adsorption/desorption technique. The results indicated that zirconia with a surface area as high as 100 m²/g can be obtained by this method after calcination at 500°C. Zirconia presents three polymorphic phases (monoclinic, tetragonal and cubic), which are reversibly interconversible. The cluster model Zr₄O₈ and Zr₄O₇ ⁺² was used for a theoretical study of the stabilization process. The ab initio RHF method was employed with the Gaussian94 program and the total energies and the energy gap of the different phases were calculated and compared with the experimental energy gap. The theoretical results show good reproducibility of the energy gap for zirconia.     

Simultaneous sulfide and acetate oxidation under denitrifying conditions using an inverse fluidized bed reactor

BACKGROUND: Simultaneous removal of sulfur, nitrogen and carbon compounds from wastewaters is a commercially important biological process. The objective was to evaluate the influence of the CH₃COO^?/NO₃^? molar ratio on the sulfide oxidation process using an inverse fluidized bed reactor (IFBR). RESULTS: Three molar ratios of CH₃COO^?/NO₃^? (0.85, 0.72 and 0.62) with a constant S^2?/NO₃^? molar ratio of 0.13 were evaluated. At a CH₃COO^?/NO₃^? molar ratio of 0.85, the nitrate, acetate and sulfide removal efficiencies were approximately 100%. The N₂ yield (g N₂ g^?1 NO₃^?‐N consumed) was 0.81. Acetate was mineralized, resulting in a yield of 0.65 g inorganic‐C g^?1 CH₃COO^?‐C consumed. Sulfide was partially oxidized to S⁰, and 71% of the S^2? consumed was recovered as elemental sulfur by a settler installed in the IFBR. At a CH₃COO^?/NO₃^? molar ratio of 0.72, the efficiencies of nitrate, acetate and sulfide consumption were of 100%, with N₂ and inorganic‐C yields of 0.84 and 0.69, respectively. The sulfide was recovered as sulfate instead of S⁰, with a yield of 0.92 g SO₄^2?‐S g^?1 S^2? consumed. CONCLUSIONS: The CH₃COO^?/NO₃^? molar ratio was shown to be an important parameter that can be used to control the fate of sulfide oxidation to either S⁰ or sulfate. In this study, the potential of denitrification for the simultaneous removal of organic matter, sulfide and nitrate from wastewaters was demonstrated, obtaining CO₂, S⁰ and N₂ as the major end products. Copyright © 2008 Society of Chemical Industry     

Use of the polymerase chain reaction in the diagnosis of leprosy

A case is described in which a pericardial branch of a nongrafted left internal mammary artery communicated directly with the distal left anterior descending artery, following saphenous vein bypass grafting. This type of collateralization following coronary artery bypass surgery seems to be very rare, and perhaps could protect the myocardium from severe ischemia.     

Generalized Nakagami-m phase crossing rate

This paper provides simple, exact, new closed-form expressions for the generalized phase crossing rate of Nakagami-m fading channels. Sample numerical results obtained by simulation are presented that validate the formulations developed here. A special case of this formulation is the Rayleigh case, whose result agrees with that obtained elsewhere in the literature. In passing, several new closed-form results concerning the statistics of the envelope, its in-phase and quadrature components, phase, and their time derivatives are obtained.     

Wake and aerodynamics loads in multiple bodies—application to turbomachinery blade rows

Two-dimensional, unsteady flow around bodies of complex geometry (or multiple bodies) at high Reynolds number is simulated using the vortex method. This method is modified to take into account the sub-grid scale phenomena through a second order velocity structure function model adapted to the Lagrangian scheme. The dynamics of the body wake is computed using the convection-diffusion splitting algorithm; the convection process is carried out with a Lagrangian Adams-Bashforth time-marching scheme and the diffusion process is simulated using the random walk method. The pressure distribution is obtained using an integral equation derived from the pressure Poisson equation, which was first developed for a single body. Results for the numerical simulation around a linear cascade of airfoils are presented. As the flow is periodic in the y direction, the discrete vortex shedding need only be considered for a reference airfoil. The flow characteristics around the NACA 65-410 series airfoils are calculated and comparisons are made with results available in the literature.     

Microstructural and textural characterization of a hot-rolled IF steel

The present paper reports the experimental results on the microstructural and textural characterization of a hot-rolled IF steel. The IF steel was hot-rolled in multiple passes in the austenitic field (1,070 °C) followed by air-cooling. SEM, TEM, and LOM were used to image the microstructure of the material. The global texture was determined by X-ray diffraction (XRD) technique. The mesotexture of selected regions was investigated by electron backscatter diffraction (EBSD). Results show the presence of a diffuse (nearly random) and weak texture in the hot-band that consists of recrystallized polygonal grains and subgrains. The fraction of boundaries with misorientations comprised in the interval 2° ≤ ψ < 15° was found to be lower than 5%. It can be concluded that these low angle boundaries and the presence of subgrains can be associated to the existence of a few areas softened by recovery during or after hot rolling in austenitic field.     

Total and acid-soluble fluoride content of infant cereals, beverages and biscuits from Brazil

Total fluoride (TF) and HCl 0.01 M ('gastric juice')-soluble fluoride (SF) were analysed in infant foods, beverages and calcium-rich biscuits. Samples were divided into seven categories: children cereals (A), chocolate-flavoured milk (B), soy beverages (C), filled biscuits (D), non-filled biscuits (E), wafer biscuits (F) and corn starch biscuits (G). Mean TF concentrations ± SD (amplitude, unit µg F ml^-1 or µg F g^-1) were: (A) 4.25 ± 3.04 (0.20 - 7.84, n = 6); (B) 0.34 ± 0.47 (0.05-1.27, n = 6); (C) 0.15 ± 0.07 (0.09-0.29, n = 8); (D) 8.44 ± 1.76 (7.65-10.47, n = 4); (E) 12.41 ± 1.15 (10.69-13.68, n = 4); (F) 0.35 ± 0 (0.34-0.36, n = 4) and (G) 7.77 ± 1.12 (6.86-8.68, n = 2). Five samples of cereals, one sample of chocolate-flavoured milk and 10 samples of biscuits were analysed for SF. In cereals analysed for SF, all fluoride was soluble, while for the chocolate-flavoured milk, approximately 50% of TF was soluble. Regarding the biscuits analysed for SF approximately 20% of TF was soluble. It was observed that some of the cereals and beverages, and most of the biscuits analysed, might be important contributors to total daily fluoride intake. When consumed just once per day, cereals and beverages might supply up to 25% of the maximum recommended daily fluoride intake (0.07 mg F kg^-1 body weight) for a 2-year-old child (12 kg). For the filled, non-filled and corn starch biscuits, when 3, 32 or 20 units of them, respectively, are consumed just once per day, they may supply up to 16% of the maximum recommended daily fluoride intake. However, only approximately 25% of fluoride absorption occurs from the stomach and 75% from the small intestine. Therefore, a higher fluoride bioavailability is possible.