The Molecular and Crystal Structure of the Glycopeptide A-40926 Aglycone

The crystal structure of a glycopeptide antibiotic A–40926 aglycone was investigated by X-ray analysis at ?120°. A-40926 crystallises in the orthorhombic space group P2₁2₁2₁ with two monomers in the asymmetric unit, a = 21.774(4), b = 28.603(7), c = 29.757(4) Å. ‘Conventional’ direct methods approach failed to solve the structure, but a novel iterative real/reciprocal space procedure was successful. Refinement against 11248 F² data led to R1 = 13.3% for 6770 F > 4σ (F). The two monomers of A-40926 have similar conformations and are bound by antiparallel H-bonds to form a ‘chain’ structure of connecting dimers. The antibiotic molecule possesses a ‘binding pocket’ for the C-terminal carboxy group of the cell-wall protein, which is consisten with suggestions based on NMR data and the recently reported crystal structure of ureido-balhimycin. In A-40926 the monomers are polymerically linked by H-bonds, quite unlike the tight dimer formation observed in ureido-balhimycin.     

3-Diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolat(II) — Synthese und Struktur

3-Diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolate(II) — Synthesis and Structure Bis-(N′, N′-diethyl-N-benzoylselenoureato)nickel(II) reacts with diphosgene in benzene to 3-diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolate(II). Its structure is confirmed by RKSA and ESCA. The compound consists of cations, which are planar fivemembered rings and of tetrahedral tetrachloroniccolate(II) anions. The complex is isomorphic with 3-diethylamino-5-phenyl-1,2,4-dithiazolium-tetrachloroniccolate(II).     

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.     

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.     

A system for defining reference materials applicable to all food matrices

Recently the subcommittee on Food Definition of the AOAC INTERNATIONAL Task Force on Methods for Nutrition Labeling proposed a Food Matrix Organizational System [4] to systematically judge the applicability of collaboratively studied methods over a range of food matrices. This system describes a food matrix by its location in one of nine sectors in a triangle, with each point of the triangle defined as representing 100% and the opposite side representing 0% of the normalized contents of each of three major components of FAT, PROTEIN and CARBOHYDRATE. Foods falling within the same sector would be chemically similar and thus should behave in a similar analytical manner. This same scheme can be used to select one or two food matrices representing each sector, for development of a series of reference materials representing all foods. The list of 5250 foods contained in the USDA Nutrient Data Base for Standard Reference has been sorted and matched to this schematic to determine the scope of the selection process. In addition the list of foods in the USDA Data Base for Food Consumption Surveys has been examined. Results and progress of this selection process are reported.