Recent applications of analytical techniques for quantitative pharmaceutical analysis: A review

The intension of this paper was to review and discuss some of the current quantitative analytical procedures which are used for quality control of pharmaceutical products. The selected papers were organized according to the analytical technique employed. Several techniques like ultraviolet/visible spectrophotometry, fluorimetry, titrimetry, electroanalytical techniques, chromatographic methods (thin-layer chromatography, gas chromatography and high-performance liquid chromatography), capillary electrophoresis and vibrational spectroscopies are the main techniques that have been used for the quantitative analysis of pharmaceutical compounds. In conclusion, although simple techniques such as UV/VIS spectrophotometry and TLC are still extensively employed, HPLC is the most popular instrumental technique used for the analysis of pharmaceuticals. Besides, a review of recent works in the area of pharmaceutical analysis showed a trend in the application of techniques increasingly rapid such as ultra performance liquid chromatography and the use of sensitive and specific detectors as mass spectrometers.

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.

Quantification of water in ethanol using a photothermal transparent transducer

Ethanol with added water may be found during the process of assessing its physical and chemical properties. This addition can damage automotive vehicle engines and also may contribute to tax evasion. The present contribution describes a method based on a photothermal transparent transducer to determine the water content in ethanol. A chamber with a window of lithium tantalate coated with a thin layer of indium tin oxide was used, and a 1450-nm laser diode was employed as the excitation source. The results indicated a nearly linear response of the apparatus, as a function of the water content in water/ethanol solutions ranging from 0 to 100 (vol.%). The results for the dependency of the photothermal signal on the laser power and chopping frequency suggested that reliable results can be obtained using laser power and chopping rates above 100 mW and 10 Hz, respectively. The results reported here may be useful in the development of an alternative method that can provide real-time data on the water concentration in ethanol in a rapid, portable and unambiguous way, and that can be easily used in laboratory analyses or in gas stations. © 2013 Elsevier B.V.

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.

Morphology of the female genital ducts of the blue land crab Cardisoma guanhumi (Crustacea: Brachyura: Gecarcinidae)

This is a histological and histochemical analysis of the terminal portion of the female reproductive system and genital ducts of the blue land crab (Cardisoma guanhumi). Animals were collected in the Jaguaribe estuary (Ceará, Brazil) and dissected. Genital duct fragments were fixed and submitted to different staining techniques. The female reproductive system consists of a pair of ovaries and a pair of genital ducts. In the mid-posterior portion of each lobe, the ovaries communicate with the genital ducts, which are subdivided into oviduct, spermatheca, vagina, and gonopore. Histologically, the spermatheca of C. guanhumi is composed of columnar secretory epithelium and is divided into a dorsal zone and a ventral zone, the latter covered internally by a cuticle layer. Both zones are enveloped by a thin layer of loose connective tissue. Histological cross sections revealed the vagina to be concave, a pattern considered phylogenetically more advanced than the simple, tubular form. Our findings suggest fertilization is internal, favoring sperm from the most recent copulation. © 2012 The Authors. Acta Zoologica © 2012 The Royal Swedish Academy of Sciences.

Isotermas de sorção e cinética de secagem de sementes de pomelo

The drying of grapefruit seeds, by-products from grapefruit processing, was studied at 40, 50, 60 and 70°C and at three air velocities, 0.6, 1.0 and 1.4 m s-1. Sorption isotherms of grapefruit seeds were obtained at each temperature by the static method using saturated salt solutions. The Henderson model adequately described the sorption isotherms, over the entire temperature range. Drying rates indicated that the drying of grapefruit seeds took place under the falling rate period. Effective moisture diffusivity in grapefruit seeds ranged from 4.36 × 10-10 to 6.82 × 10-10 m2 s-1. The temperature dependence of the effective diffusivity followed an Arrhenius relationship, and the activation energies were 12.23, 11.29 and 11.79 kJ mol-1 for dried grapefruit seeds under air velocities of 0.6, 1.0 and 1.4 m s-1, respectively. Three thin-layer models were used to predict the drying curves, Page, Lewis, and Henderson-Pabis model. The Page model presented the best fit for all drying air temperatures and velocities studied.

Uso do sistema de cultivo bidimensional e tridimensional para diferenciação de células-tronco espermatogoniais e indução da espermatogênese in vitro em murinos

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Caracterização química, microbiológica e farmacognóstica da polpa de coquinho-azedo (Butia capitata (Mart) Becc) produzida em Arinos-MG

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Emprego de membrana de celulose microfibrilar na ceratoplastia lamelar em coelhos (O. cuniculus, Linnaeus, 1758): aspectos clínicos, morfológicos e imunoistoquimicos

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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)

Análise químico-farmacêutica de cefazolina sódica em pó liofilizado para solução injetável

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Estudo farmacognóstico e desenvolvimento de fitocosmético de ação antioxidante dos frutos de Dimorphandra mollis Benth. (Leguminosae-Caesalpinioideae)

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Desenvolvimento e controle de qualidade de formulação cosmética contendo digluconato de clorexidina

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estudo fitoquímico, avaliação da atividade antimicrobiana, antioxidante e citotóxica de extrativos de Equisetum hyemale L. (Equisetaceae)

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)