Synthesis of homoceramides, novel ceramide analogues, and their lack of effect on the growth of hippocampal neurons

The synthesis of a new series of D-erythro-homoceramide analogues is described. Several synthetic approaches were investigated. Homoceramides can be successfully synthesized from L-homoserine as chiral building block and a protected Weinreb-amide as a key intermediate. The synthesis of short-chain analogues with a heptyl side chain, as well as with a phenyl residue in the sphingoid part (instead of the naturally occurring tridecyl side chain), was effected. The homoceramides 15-17 and 24 were investigated for their potential to reverse the inhibitory effect of fumonisin B(1) on axonal growth. Unfortunately, none of the tested compounds showed any biological activity due to their lack of metabolism to glucosylhomoceramide.     

Co(II)5(OH)6(SO4)2(H2O)4: the first ferromagnet based on a layered cobalt-hydroxide pillared by inorganic...OSO3-Co(H2O)4-O3SO..

The synthetic mineral Co(II)5(OH)6(SO4)2(H2O)4 (1), obtained by hydrothermal reaction of CoSO4.7H2O and NaOH at 165 degrees C and consisting of brucite-like Co4(OH)6O2 layers pillared by OSO3-Co(H2O)4-O3SO, is a ferromagnet (T(Curie)= 12 K, Hc= 580 Oe).     

Synthesis and Characterization of Novel Polyimides Based on Pyridine-containing Diamine

A new aromatic diamine monomer containing pyridine unit, 2,6-bis （4-aminophenoxy- 4＇-benzoyl）pyridine（BABP）, was synthesized in three steps, starting from 2,6-pyridinedicarboxyl chloride. A series of novel pyridine-containing polyimides were prepared v/a the polycondensation of BABP with various aromatic dianhydrides through poly（amic acid） precursors, and thermal or chemical imidization of the precursors. The polyimides exhibit desirable properties, e.g., good solubility in N-methyl-2-pyrrolidone and m-cresol, excellent thermal stability and film-forming capability, as well as high inherent viscosity, indicating high molecular weight.     

Synthesis, nuclear, and magnetic structures and magnetic properties of [Mn3(OH)2(SO4)2(H2O)2

[Mn(3)(OH)(2)(SO(4))(2)(H(2)O)(2)] and its deuterated analogue were synthesized by a hydrothermal technique and characterized by differential thermal analysis, thermogravimetric analysis, and IR spectroscopy. Its nuclear structure, determined by single-crystal X-ray analysis and Rietveld analysis of neutron powder-diffraction data, consists of a 3D network of chains of edge-sharing Mn(1)O(6), running along the c axis, connected by the apices of Mn(2)O(6) and SO(4) units. It is isostructural to the nickel analogue. Determination of the magnetic structure and measurements of magnetization and heat capacity indicate the coexistence of both magnetic long-range ordering (LRO) and short-range ordering (SRO) below a Néel temperature of 26 K, while the SRO is retained at higher temperatures. The moments of the two independent Mn atoms lie in the bc plane, and that of Mn(1) rotates continuously by 54 degrees towards the c axis on decreasing the temperature from 25 to 1.4 K. While the SRO may be associated with frustration of the moments within a Mn(3) trimer, the LRO is achieved by antiparallel alignment of the four symmetry-related trimers within the magnetic unit cell. A spin-flop field, measured by dc and ac magnetization on a SQUID, is observed at 15 kOe.     

Preliminary characterization of anhydrous ethanol used in Brazil as automotive fuel

This work reports preliminary studies on the characterisation of anhydrous ethanol (AEA) used as an automotive fuel mixed with gasoline in Porto Alegre (South Brazil). Pre-concentration of the impurities contained in 1000 ml of AEA was carried on through solid-phase extraction using XAD4 resin. The main compounds in the extract were identified by means of spectral data from the library of the equipment. The concentrate was then fractionated using a preparative liquid chromatographic column filled with activated silica gel and the elution procedure was carried out with, n-hexane, n-hexane-benzene (1:1, v/v) and dichloromethane. Prior to analysis by GC-MS, each fraction was reduced to 1 ml with a gentle stream of nitrogen. Saturated linear hydrocarbons and aromatic hydrocarbons eluted in the first fraction and oxygenated compounds such as aldehydes. ketones and alcohols, eluted in the second one. were the main compounds detected in the sample.     

Determination of moxifloxacin in tablets and human urine by square-wave adsorptive voltammetry

This work presents an electroanalytical methodology developed for square-wave voltammetry based in the electrochemical reduction in hanging mercury drop electrode (HMDE), which is simple, fast, reliable and sensitive for determination of moxifloxacin (MOXI) in tablets and spiked urine human samples. The support electrolyte that provided a more defined and intense peak current for MOXI determination was the phosphate buffer 0.04 mol l^{− 1} pH 8.0. In the best-optimized conditions the drug presented an only peak of reduction at − 1.38 V vs. Ag/AgCl, using an E_acc. of − 0.30 V. An LOD of 0.44 and 3.20 ng ml^{− 1} and an LOQ of 1.46 and 10.60 ng ml^{− 1} were found for the pure standard of moxifloxacin and in the presence of matrix, respectively. A good recovery was obtained for assay spiked urine samples and a good quantification of MOXI was achieved in a commercial formulation. The methodology proposed was more sensitive than the spectrofluorimetric and spectrophotometric method with precision and accuracy equivalent.     

Cloud point extraction of vanadium in parenteral solutions using a nonionic surfactant (PONPE 5.0) and determination by flow injection-inductively coupled plasma optical emission spectrometry

A preconcentration and determination methodology for vanadium at trace levels in parenteral solutions was developed. Cloud point extraction was successfully employed for the preconcentration of vanadium prior to inductively coupled plasma atomic optical emission spectrometry (ICP-OES) coupled to a flow injection (FI) system. The vanadium was extracted as vanadium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol [V-(5-Br-PADAP)] complex, at pH 3.7 mediated by micelles of the nonionic surfactant polyoxyethylene (5.0) nonylphenol (PONPE 5.0). The extracted surfactant-rich phase (100 mul) was mixed with 100 mul of ethanol and this final volume injected into ICP-OES for the vanadium determination. Under these conditions, the 50 ml sample solution preconcentration allowed raising an enrichment factor of 250-fold; however, it was possible to obtain a theoretical enrichment factor of 500-fold. The lower limit of detection (LOD) obtained under the optimal conditions was 16 ng l(-1). The precision for 10 replicate determinations at the 2.0 mug l(-1) V level was 2.3% relative standard deviation (RSD), calculated with the peak heights. The calibration graph using the preconcentration system for vanadium was linear with a correlation coefficient of 0.9996 at levels near the detection limits up to at least 50 mug l(-1). The method was successfully applied to the determination of vanadium in parenteral solution samples.     

Adaptive efficient analysis for big data ergodic diffusion models

Statistical Inference for Stochastic Processes - We consider drift estimation problems for high dimension ergodic diffusion processes in nonparametric setting based on observations at discrete...     

A dominance-based rough set approach applied to evaluate the credit risk of sovereign bonds

4OR - Even though sovereign bonds represent low-risk alternatives that give investors a healthy income, the risk assessment process for these bonds is still considered subjective because of the...     

The inclusion of rhodium(II)α-methyl-cinnamate in β-cyclodextrin

The preparation and characterization of the 1:1 inclusion compound of rhodium(II) -methyl cinnamate in -cyclodextrin is reported. Evidence of inclusion was obtained from X-ray powder diffraction results, Raman, IR and UV-Vis spectroscopic studies and thermal analysis. Given the potential antitumor activity of the rhodium(II) carboxylate and its virtual insolubility in water, its inclusion in -cyclodextrin opens the possibility for its transference to the aqueous phase.