Determination of oligoelements in parenteral formulations by planar chromatography and spectrophotometry

The authors have studied the chromatographic behavior of parenteral preparations for pediatric use containing inorganic cations. After separation and identification by thin-layer chromatography, Mn2+, Zn2+, and Cu2+ were analyzed by a method based on reaction with an appropriate reagent and extraction with an organic solvent which yielded elution and preconcentration, resulting in an appropriate solution for colorimetric quantitation. Cr3+ cation was determined by atomic absorption spectrophotometry after appropriate chromatographic separation, using microcrystalline cellulose (adsorbent) and an acetone:water:hydrochloric acid mixture (80:5:8) as the mobile phase.

Robust state-derivative feedback LMI-based designs for multivariable linear systems

In some practical problems, for instance in the control systems for the suppression of vibration in mechanical systems, the state-derivative signals are easier to obtain than the state signals. New necessary and sufficient linear matrix inequalities (LMI) conditions for the design of state-derivative feedback for multi-input (MI) linear systems are proposed. For multi-input/multi-output (MIMO) linear time-invariant or time-varying plants, with or without uncertainties in their parameters, the proposed methods can include in the LMI-based control designs the specifications of the decay rate, bounds on the output peak, and bounds on the state-derivative feedback matrix K. These design procedures allow new specifications and also, they consider a broader class of plants than the related results available in the literature. The LMIs, when feasible, can be efficiently solved using convex programming techniques. Practical applications illustrate the efficiency of the proposed methods.

AN ISOCOUMARIN DERIVATIVE FROM PAEPALANTHUS BROMELIOIDES

The structure of 5,7,9,10-tetramethoxy-3-methyl-1 H-naphtho[2,3-c]pyran-1-one, C18H18O6, a derivative of a natural isocoumarin isolated from Paepalanthus bromelioides, was determined by X-ray analysis, which unequivocally confirmed the previously assigned structure. Small deviations from the standard angles, resulting from steric hindrance between the methoxyl and carbonyl groups, were observed.

Thermal and photochemical stability of poly(vinyl alcohol)/modified lignin blends

A kraft lignin derivative (KLD) obtained by reaction with p-aminobenzoic acid/phthalic anhydride was blended with poly(vinyl alcohol) (PVA) by solution casting from DMSO. PVA and PVA/KLD films were exposed to ultraviolet radiation (24, 48, and 96 h) and analyzed by thermogravimetry (TG), differential scanning calorimetry (DSC), infrared spectroscopy (FTIR), hydrogen nuclear magnetic resonance (H-1 NMR) spectroscopy, and scanning electron microscopy (SEM). PVA films show a loss of thermal stability due to irradiation. PVA/KLD reveals greater thermal stability than PVA and an increase in thermal stability after irradiation. These results suggest that the incorporation of KLD into PVA provides a gain in thermal and photochemical stability. FTIR, H-1 NMR, DSC, and TG results obtained for the blends suggest that intermolecular interactions between PVA and KLD chains are present. SEM micrographs revealed blend miscibility for a KLD blend content of up to 15 wt%, as observed at magnification of 1000 times. (c) 2005 Elsevier Ltd. All rights reserved.

Measurement of low-derivative surface lenses by two-laser holography with Bi12TiO20 crystals

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Electrochemistry of organometallic compounds. Part III. Oxidations of methyl derivatives of organocobalt(III) complexes with delocalized electronic structure in dimethylformamide

The influence of the equatorial ligand on the electrochemical oxidation of the compounds [H3CCo(chel)B], where chel is bis (dimethylglyoximato), (DH)2; bis(salicylaldehyde)ethylenediimine, salen; bis(salicylaldehyde) o-phenylenediimine, salophen; bis(salicylaldehyde)cyclohexylenediimine, salcn; bis(acetylacetone) ethylenediimine, bae; and where B is pyridine when chel is (DH2), and dimethylformamide (DMF) when chel represents a Schiff base (salen, salcn, salophen and bae), was studied by means of cyclic voltammetry in DMF, 0.2 M in tetraethylammonium perchlorate, between 25 and -25°C, with a platinum disk working electrode. Absorption spectra in the visible and near ultraviolet regions for these compounds in DMF at 25°C were obtained. The complexes exhibit a reversible one-electron oxidation, at -20°C with scan rates >0.5 V s-; chemical reactions following electron transfer are not detected under these conditions. At slower potential or higher temperatures, the oxidized product decomposes chemically in a solvent-assisted (or nucleophile-assisted) reaction, yielding products which are electroactive in the applied potential range. The behavior of the [H3CCo (DH2)py] derivative is better described as a quasi-reversible charge transfer followed by an irreversible chemical reaction. Experimental evidence suggests that in the case of the [H3CCo(bae)] derivative at -20°C, the reactive -species is pentacoordinated and weakly adsorbed at the electrode surface. The value of E 1 2 and the energies of the first two absorption bands in the visible spectra reveal the ability of the studied complexes to donate and to delocalize electronic charge. © 1982.

Methyl(2-mercapto-4-methylpyrimidinato)mercury(II): A methylmercury(II) derivative with an unusual metal-metal interaction

4-Methylpyrimidine-2-thione reacts with methylmercury hydroxide to give the thiolate derivative HgMe(SC4H2N2Me-2), the X-ray structure of which reveals pairs of molecules with a mercury-mercury distance of 3.10 Å.

ESTABILIDADE TERMICA DO PARACETAMOL EM SOLUCAO: CROMATOGRAFIA EM CAMADA DELGADA (CCD) - ESPECTROFOTOMETRIA ULTRAVIOLETA

The interference practised by the products in degradation of paracetemol when there is the application of spectrophotometry UV is the main obstruction to the execution of studies of thermic stability. The application of chromatography in slender layer to the isolation of paracetamol, besides being the excessively hard to apply was satisfactory to the desired proposal. The type and extension of degradation suffered by paracetamol in solution suggest the convenient inclusion, in the formulations, of one system antioxidant. This practice makes possible the blockage of the oxidation of p-aminophenol, produced by the hydrolytic degradation of paracetamol; this fact propitiated the diminution of the number of products of degradation in the medicine, making the use more secure. On the other hand, considering especially the methodological necessities of the present work, the presence of one antioxidant system facilitated the separation of paracetamol through the Thin Layer Chromatography and consequently optimized its quantification by Spectrophotometry UV during the study of thermic stability. The formulation proposed revealed excellent stability.

The Effects of N Helix Deletion and Mutant F29W on the Ca2+ Binding and Functional Properties of Chicken Skeletal Muscle Troponin C

To assess the structural and functional significance of the N helix (residues 3-13) of avian recombinant troponin C (rTnC), we have constructed NHdel, in which residues 1-11 have been deleted, both in rTnC and in the spectral probe mutant F29W (Pearlstone, J. R., Borgford, T., Chandra, M., Oikawa, K., Kay, C. M., Herzberg, O., Moult, J., Herklotz, A., Reinach, F. C., and Smillie, L.B. (1992) Biochemistry 31, 6545-6553). Comparison of the far- and near-UV CD spectra (±Ca2+) of F29W and F29W/ NHdel and titration of the Ca2+-induced ellipticity and fluorescence changes indicates that the deletion has little effect on the global fold of the molecule but reduces the Ca2+ affinity of the N domain, but not the C domain, by 1.6-1.8-fold. Comparisons of the mutants NHdel, F29W, and F29W/NHdel with rTnC have been made using several functional assays. In reconstituted troponin-tropomyosin actomyosin subfragment 1 and myofibrillar ATPase systems, both F29W and NHdel have significantly reduced Ca2+-activated enzymic activities. These effects are cumulative in the double mutant F29W/ NHdel. On the other hand, maximal isometric tension development in Ca2+-activated reconstituted skinned fibers is not affected with F29W and NHdel, although the Ca2+ sensitivity of NHdel in this system is markedly reduced. We conclude that both mutations, NHdel and F29W, are functionally deleterious, possibly affecting interactions of the N domain with troponin I and/or T.

Consistent higher derivative quantum field theory: A model without tachyons and ghosts

We present a higher derivative gauge theory in (2 + 1) dimensions which can have its parameters suitably tuned in order to become a consistent quantum field theory, in the sense that both tachyons and ghosts are absent from the particle spectrum of the theory.

Continuous wave ultraviolet frequency upconversion due to triads of Nd3+ ions in fluoroindate glass

We have observed ultraviolet upconversion fluorescence from the 4D3/2 and 2P3/2 levels of Nd3+ in fluoroindate glass under infrared pumping. It was found that the excitation of a large population in the 4F3/2 metastable level allows to achieve strong upconversion emissions at 354 and 382 nm. A simple rate equation model reproduces the temporal behavior of the upconverted emission and allows us to estimate the energy transfer rate among three Nd3+ ions participating in the process. © 1997 American Institute of Physics.

Fermion helicity flip in higher-derivative electromagnetism

It is shown that massive fermions have their helicity flipped on account of their interaction with an electromagnetic field described by Podolsky's generalized electrodynamics. Massless fermions, in turn, seem to be unaffected by the electromagnetic field as far as their helicity is concerned. © Springer-Verlag 1997.

HPLC determination of flumethrin, deltamethrin, cypermethrin, and cyhalothrin residues in the milk and blood of lactating dairy cows

A procedure to determine residue concentrations of synthetic pyrethroid insecticides (flumethrin, deltamethrin, cypermethrin and cyhalothrin) in the milk and blood of lactating dairy cows was developed. Extraction was performed with acetonitrile, n-hexane partitioning, and silica gel column cleanup with n-hexane and diethyl ether. Analysis was carried out by high- performance liquid chromatography and ultraviolet detection. Recovery of the four pyrethroids averaged 78 to 91% with a minimum detectable concentration of 0.001 mg/kg. The method was reproducible and sensitive.

Electrochemical behavior of a nitrobenzenesulfonyl derivative of aniline in aqueous solution

The electrochemical behavior of aniline protected by a nitrobenzene sulphonyl group in aqueous solution at a mercury electrode is reported. At pH < 10 the compound was reduced in a single well-defined step. Reduction of the nitro group involving a preceding protonation step was postulated. Two reduction steps are present at higher pH (pH > 11). Controlled potential electrolysis confirms that the reduction of the nitro group in a four-electron step to N-phenyl-4-hydroxylamine sulphonamide is always the preponderant process. ©1997 Soc. Bras. Química.