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.

Thermal decomposition of acetylsalicylic acid (aspirin)

The thermal decomposition of aspirin in air and dry air flux was investigated. Thermogravimetry-derivative thermogravimetry (TG-DTG), differential scanning calorimetry (DSC), nuclear magnetic resonance (NMR), infrared absorption spectra and thin layer chromatography have been used to study the thermal decomposition of this compound. The results permit the identification of some compounds revealed in the first step of the TG-DTA curves, and also suggest the thermal decomposition mechanism.

Isolation of ergosterol peroxide and its reversion to ergosterol in the pathogenic fungus Sporothrix schenckii

Ergosterol peroxide, a presumed product of the H2O2-dependent enzymatic oxidation of ergosterol, has been isolated from yeast from yeast forms of the pathogenic fungus Sporothrix schenckii. The substance, which may have a role in fungal virulence, has been characterized mainly using spectroscopic methods (1H and 13C nuclear magnetic resonance and high resolution mass spectra). The purified compound showed a molecular formula of C28H44O3, displaying characteristic features of epidioxy sterols and was reverted to ergosterol when submitted to S. schenckii enzymatic extract.

A new cytotoxic naphthopyrone dimer from Paepalanthus bromelioides

A new naphthopyrone dimer was isolated from the capitula of Paepalanthus bromelioides by chromatographic procedures. Its structure was deduced from spectrometric data. On colorimetric assay for cytotoxicity the new dimer showed IC50 of 55.9 μM. (C) 2000 Elsevier Science B.V.

Ativação de macrófagos por produtos naturais obtidos da Achillea millefolium L. (Asteraceae)

Plants are a valuable source of natural products for the maintenance of human health. The purpose of this paper was the study of immunologic activity of yarrow (Achillea millefolium L.), a largely used plant in popular medicine that has many different properties such as: antiinflammatory, astringent, antiseptic and antispasmodic. Macrophages stimulation was evaluated by the determination of H2O2, NO and TNF-α in supernatants of peritoneal macrophages cultures of mice in the presence of the yarrow leaves extract. The thin layer chromatography of extract was also analyzed, showing rutin. All concentrations showed a moderate release of H2O2 and the concentrations of 6, 8 and 10mg/mL had a higher release of NO. The TNF-a was produced in all concentrations, but the best result was obtained at 4mg/mL. Analyzing the results, it is suggested that the yarrow ethanolic extract can modulate the macrophages activation.

Determinação de fármacos diuréticos em associação por cromatografia em camada delgada e espectrofotometria

A rapid, sensitive and reliable thin-layer chromatography/spectrophotometry screening procedure was developed for quantitative determination of diuretics associated in pharmaceutical dosage forms. The chromatographic method employed microcrystalline cellulose and butanol : acetic acid : water (4:1:1) or amilic alcohol : ammonium hydroxide 25% (9:1) as mobile phases and detection by U.V. light. The drugs were extracted using a simple procedure and were quantified by U.V. spectrophotometry. Results varied from 97.5 to 102.5% and are similar to those obtained by conventional methods. This method of quantification of diuretics is promising for quality control of drugs.

Identificação de diterpenos clerodânicos em diferentes órgãos de Casearia sylvestris Swartz

Casearia sylvestris Swartz (Salicaceae) is a tree or shrub distributed widely in Brazil, where it is used in popular medicine. Several bioactive clerodane diterpenes typical of Casearia have been isolated from this species (e.g. casearins and casearvestrins). The main objective of this study was to identify clerodane diterpenes in various organs of C. sylvestris, using chromatographic and spectroscopic analytical techniques. The extracts of the different plant parts were analyzed by thin layer chromatography, high performance liquid chromatography with diode array detector and 1H nuclear magnetic resonance. In the chromatographic analysis, clerodane diterpenes isolated from C. sylvestris were used as standards, including rel-19Sacetóxi-18R- butanoilóxi-18,19- epóxi -6S -hidróxi -2R-(2-metilbutanoilóxi) -5S, 8R, 9R, 10S -cleroda-3,13(16),14-triene, isolated for the first time from the stems. Phytochemical profiles of the organs were produced, which indicated the presence of clerodane diterpenes in all parts of the plant, notably in the leaves. The results also suggest that the main clerodane diterpenes in the stems, flowers and roots had conjugated double-bond patterns that differed from those found in the leaves.

rastreamento histoquímico, fitoquímico e biológico de folhas de Plinia cauliflora (DC.) Kausel (Myrtaceae)

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Structural characterization of a new dextran with a low degree of branching produced by Leuconostoc mesenteroides FT045B dextransucrase

This paper offers the physical and chemical characterization of a new dextran produced by Leuconostoc mesenteroides FT045B. The chemical structure was determined by Fourier Transform Infrared spectroscopy and 1H Nuclear Magnetic Resonance spectroscopy. The dextran was hydrolyzed by endodextranase; the products were analyzed using thin layer chromatography and compared with those of commercial B-512F dextran. The number-average molecular weight and degree of polymerization of the FT045B dextran were determined by the measurement of the reducing value using the copper bicinchoninate method and the measurement of total carbohydrate using the phenol-sulfuric acid method. The data revealed that the structure of the dextran synthesized by FT045B dextran sucrase is composed of d-glucose residues, containing 97.9% α-(1,6) linkages in the main chains and 2.1% α-(1,3) branch linkages compared with the commercial B-512F dextran, which has 95% α-(1,6) linkages in the main chains and 5% α-(1,3) branch linkages. © 2012 Elsevier Ltd. All rights reserved.

Fontes de carbono de baixo custo para a produção de xilanase termoestável por aspergillus niger

A strain of the flamentous fungus Aspergillus niger was isolated and shown to possess extracellular xylanolytic activity. These enzymes have biotechnological potential and can be employed in various industries. This fungus produced its highest xylanase activity in a medium made up of 0.1% CaCO3, 0.5% NaCl, 0.1% NH4Cl, 0.5% corn steep liquor and 1% carbon source, at pH 8.0. A low-cost hemicellulose residue (powdered corncob) proved to be an excellent inducer of the A. niger xylanolytic complex. Filtration of the crude culture medium with suspended kaolin was ideal for to clarify the extract and led to partial purifcation of the xylanolytic activity. The apparent molecular mass of the xylanase was about 32.3 kDa. Maximum enzyme activity occurred at pH 5.0 and 55-60oC. Apparent Km was 10.41 ± 0.282 mg/mL and Vmax was 3.32 ± 0.053 U/mg protein, with birchwood xylan as the substrate. Activation energy was 4.55 kcal/mol and half-life of the crude enzyme at 60oC was 30 minutes. Addition of 2% glucose to the culture medium supplemented with xylan repressed xylanase production, but in the presence of xylose the enzyme production was not affected.

Desenvolvimento de métodos analíticos qualitativos para a análise de darunavir comprimidos

Darunavir is a protease inhibitor used in the treatment of HIV infection. It is a pillar of the drug cocktail for patients diagnosed with the virus. Quality control in the pharmaceutical industry, to verify the content of active substance and study the physicochemical characteristics of the drug, is essential to ensure final product quality. Until now, standardized methods for the analysis of darunavir have not been available in official compendia. This justifies new research, to develop and validate analytical methods, as well as physicochemical and pharmaceutical analysis for this drug, both as a raw material and a finished product. Thus, in this study, (a) the average weight of darunavir tablets and (b) the melting point of the pure drug were determined, and the following analytical techniques were performed: (c) thin-layer chromatography, (d) ultraviolet spectroscopy, (e) infrared spectroscopy and (f) high performance liquid chromatography. By developing the above techniques, it is possible to make a qualitative assessment of the quality of darunavir tablets.

Antineoplásico potencial: síntese de derivado de salicilato de octila e5-fluoruracila para tratamento do câncer de pele

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)