Development of a fast capillary electrophoresis method for the determination of propranolol-Total analysis time reduction strategies

The aim of this study was to develop a fast capillary electrophoresis method for the determination of propranolol in pharmaceutical preparations. In the method development the pH and constituents of the background electrolyte were selected using the effective mobility versus pH curves. Benzylamine was used as the internal standard. The background electrolyte was composed of 60 mmol L(-1) tris(hydroxymethyl)aminomethane and 30 mmol L(-1) 2-hydroxyisobutyric acid,at pH 8.1. Separation was conducted in a fused-silica capillary (32 cm total length and 8.5 cm effective length, 50 mu m I.D.) with a short-end injection configuration and direct UV detection at 214 nm. The run time was only 14 s. Three different strategies were studied in order to develop a fast CE method with low total analysis time for propranolol analysis: low flush time (Lflush) 35 runs/h, without flush (Wflush) 52 runs/h, and Invert (switched polarity) 45 runs/h. Since the three strategies developed are statistically equivalent, Mush was selected due to the higher analytical frequency in comparison with the other methods. A few figures of merit of the proposed method include: good linearity (R(2) > 0.9999); limit of detection of 0.5 mg L(-1): inter-day precision better than 1.03% (n = 9) and recovery in the range of 95.1-104.5%. (C) 2009 Elsevier B.V. All rights reserved.

Reduction of NO by CO on Cu/ZrO(2)/Al(2)O(3) catalysts: Characterization and catalytic activities

ZrO(2), gamma-Al(2)O(3) and ZrO(2)/gamma-Al(2)O(3)-supported copper catalysts have been prepared, each with three different copper loads (1, 2 and 5 wt%), by the impregnation method. The catalysts were characterized by nitrogen adsorption (BET), X-ray diffraction (XRD), temperature programmed reduction (TPR) with H(2), Raman spectroscopy and electronic paramagnetic resonance (EPR). The reduction of NO by CO was studied in a fixed-bed reactor packed with these catalysts and fed with a mixture of 1% CO and 1% NO in helium. The catalyst with 5 wt% copper supported on the ZrO(2)/gamma-Al(2)O(3) matrix achieved 80% reduction of NO. Approximately the same rate of conversion was obtained on the catalyst with 2 wt% copper on ZrO(2). Characterization of these catalysts indicated that the active copper species for the reduction of NO are those in direct contact with the oxygen vacancies found in ZrO(2). (C) 2009 Published by Elsevier Ltd.

An electroanalytical application of 2-aminothiazole-modified silica gel after adsorption and separation of Hg(II) from heavy metals in aqueous solution

2-Aminothiazole covalently attached to a silica gel surface was prepared in order to obtain an adsorbent for Hg(II) ions having the following characteristics: good sorption capacity, chemical stability under conditions of use, and, especially, high selectivity. The accumulation voltammetry of mercury(II) was investigated at a carbon paste electrode chemically modified with silica gel functionalized with 2-aminothiazole (SIAMT-CPE). The repetitive cyclic voltammogram of mercury(II) solution in the potential range -0.2 to + 0.6 V versus Ag/AgCl (0.02 mol L-1 KNO3; V = 20 mV s(-1)) show two peaks one at about 0.1 V and other at 0.205 V. The anodic wave peak at 0.205 V is well defined and does not change during the cycles and it was therefore further investigated for analytical purposes using differential pulse anodic stripping voltammetry in differents supporting electrolytes. The mercury response was evaluated with respect to pH, electrode composition, preconcentration time, mercury concentration, cleaning solution, possible interferences and other variables. The precision for six determinations (n = 6) of 0.02 and 0.20 mg L-1 Hg(II) was 4.1 and 3.5% (relative standard deviation), respectively. The detection limit was estimated as 0.10 mu g L-1 mercury(II) by means of 3:1 current-to-noise ratio in connection with the optimization of the various parameters involved and using the highest-possible analyser sensitivity. (c) 2006 Elsevier Ltd. All rights reserved.

Africanized honey bee (Apis mellifera) venom profiling: Seasonal variation of melittin and phospholipase A(2) levels

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

Perfil radial e uniformidade de precipitação do aspersor NaanDanJain 427, em função da regulagem do defletor

The study aimed to evaluate the radial profile and the uniformity of water distribution of sprinkler manufactured by the company NaanDanJain, model 427 1/2 '' M and nozzle with 2.8 mm of internal diameter, operating at pressures of 150, 200, 300 and 400 kPa and five positions of the deflector (0, 20, 50, 80 and 100%). For the determination of the parameters evaluated, the grid method was used and with the help of computer application CATCH 3D, overlapping layers of water depths was calculated with ten spacing. The results show that the deflector adjustment influences the radius of wetness and the distribution profile while the uniformity of water application showed as an important mechanism, since it permits different behavior for the sprinkler, ensuring wide track of utilization of the equipment.

Parâmetros genéticos para idade ao primeiro parto estimados por diferentes modelos para rebanhos da raça Nelore

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

Rapid and Selective UV Spectrophotometric Method for the Analysis of Ceftazidime

A new UV spectrophotometric method was developed for quantitative evaluation of ceftazidime preparations. The UV detector was set at 255 nm. Beer's law is obeyed in the concentration range of 7.0-14.0 mu g/mL. The method was found to be selective, linear, accurate, and precise in the specified ranges. Intra- and interday variability for the method were <2% relative standard deviation. Common excipients used as additives in pharmaceutical preparations do not interfere with the proposed method. This method was successfully used for quantification of ceftazidime in pure form and in pharmaceutical preparations.

Study on soluble heavy metals with preconcentration by using a new modified oligosilsesquioxane sorbent

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

Estudo da digestão de sedimento de curtume visando a extração do cromo por microemulsão

Leather tanneries generate effluents with high content of heavy metals, especially chromium, which is used in the mineral tanning process. Microemulsions have been studied in the extraction of heavy metals from aqueous solutions. Considering the problems related with the sediment resulting from the tanning process, due to its high content in chromium, in this work this sediment was characterized and microemulsion systems were applied for chromium removal. The extraction process consists in the removal of heavy metal ions present in an aqueous feeding solution (acid digestion solution) by a microemulsion system. First three different solid sludge digestion methods were evaluated, being chosen the method with higher digestion capacity. For this digestion method, seeking its optimization, was evaluated the influence of granule size, temperature and digestion time. Experimental results showed that the method proposed by USEPA (Method A) was the most efficient one, being obtained 95.77% of sample digestion. Regarding to the evaluated parameters, the best results were achieved at 95°C, 14 Mesh granule size, and 60 minutes digestion time. For chromium removal, three microemulsion extraction methods were evaluated: Method 1, in a Winsor II region, using as aqueous phase the acid digestion solution; Method 2, in a Winsor IV region, being obtained by the addition of the acid digestion solution to a microemulsion phase, whose aqueous phase is distilled water, until the formation of Winsor II system; and Method 3, in a Winsor III region, consisting in the formation of a Winsor III region using as aqueous phase the acid digestion solution, diluted in NaOH 0.01N. Seeking to optimize the extraction process only Method 1 (Systems I, II, and VIII) and Method 2 (System IX) were evaluated, being chosen points inside the interest regions (studied domains) to study the influence of contact time and pH in the extraction percentiles. The studied systems present the following compositions: System I: Surfactant Saponified coconut oil, Cosurfactant 1-Butanol, Oil phase Kerosene, Aqueous phase 2% NaCl solution; System II: Aqueous phase Acid digestion solution with pH adjusted using KOH (pH 3.5); System VIII: Aqueous phase - Acid digestion solution (pH 0.06); and System IX Aqueous phase Distilled water (pH 10.24), the other phases of Systems II, VIII and IX are similar to System I. Method 2 showed to be the more efficient one regarding chromium extraction percentile (up to 96.59% - pH 3.5). Considering that with Method 2 the microemulsion region only appears in the Winsor II region, it was studied Method 3 (System X) for the evaluation and characterization of a triphasic system, seeking to compare with a biphases system. System X is composed by: Surfactant Saponified coconut oil, Cosurfactant 1-Butanol, Oil phase Kerosene, Aqueous phase Acid digestion solution diluted with water and with its pH adjusted using 0.01N NaOH solution. The biphasic and triphasic microemulsion systems were analyzed regarding its viscosity, extraction efficiency and drop effective diameter. The experimental results showed that for viscosity studies the obtained values were low for all studied systems, the diameter of the drop is smaller in the Winsor II region, with 15.5 nm, reaching 46.0 nm in Winsor III region, being this difference attributed to variations in system compositions and micelle geometry. In chromium extraction, these points showed similar results, being achieved 99.76% for Winsor II system and 99.62% for Winsor III system. Winsor III system showed to be more efficient due to the obtaining of a icroemulsion with smaller volume, with the possibility to recover the oil phase in excess, and the use of a smaller proportion of surfactant and cosurfactant (C/S)

Avaliação mecânica in vitro utilizando miniplacas quadradas e retangulares do sistema 2.0 mm em fraturas da região anterior de mandíbula

The aim of this study was to comparatively evaluate the mechanical strength of squared and rectangular 2.0 mm system miniplates comparing them to the standard configuration with 2 straight miniplates in stabilizing fractures in the anterior mandible. Ninety synthetic polyurethane mandible replicas were used in mechanical test. The samples were divided into six groups of three different methods for fixation. Groups 1, 2 and 3 showed complete fractures in symphysis, characterized by a linear separation between the medial incisor, and groups 4, 5 and 6 showed complete fractures in parasymphysis with oblique design. Groups 1 and 4 were represented by the standard technique with two straight miniplates parallel to each other. Groups 2 and 5 were stabilized by squared miniplates and groups 3 and 6 were fixed by rectangular design. Each group was subjected to a mechanical test at a displacement speed of 10 mm/min on a universal testing machine, receiving linear vertical load on the region of the left first molar. The values of the maximum load and when displacements reached 5 mm were obtained and statistically analyzed by calculating the confidence interval of 95%. Fixation systems using squared (G2) and rectangular (G3) miniplates obtained similar results. No statistically significant differences with respect to the maximum load and the load at 5 mm displacement were found when compared to standard method in symphyseal fractures (G1). In parasymphysis the fixation method using squared miniplates (G5) obtained results without significant differences regarding the maximum load and the load at 5 mm when compared to the standard configuration (G4). The fixation method using rectangular miniplates (G6) showed inferior results which were statistically significant when compared to the standard configuration (G4) for parasymphysis fractures. The mechanical behavior of the fixation methods was similar, except when rectangular miniplates were used. The fixation methods showed better results with statistical significance in symphyseal fractures

Diagnóstico da degradação ambiental no município de Areia Branca-RN por geotecnologias

The municipality of Areia Branca is within the mesoregion of West Potiguar and within the microregion of Mossoró, covering an area of 357,58 km2. Covering an area of weakness in terms of environmental, housing, together with the municipality of Grossos-RN, the estuary of River Apodi-Mossoró. The municipality of Areia Branca has historically suffered from a lack of planning regarding the use and occupation of land as some economic activities, attracted by the extremely favorable natural conditions, have exploited their natural resources improperly. The aim of this study is to quantify and analyze the environmental degradation in the municipality. Thus initially was performed a characterization of land use using remote sensing, geoprocessing and geographic information system GIS in order to generate data and information on the municipal scale, which may serve as input to the environmental planning and land use planning in the region. From this perspective, were used a Landsat 5 image TM sensor for the year 2010. In the processing of this image was used SPRING 5.2 and applied a supervised classification using the classifier regions, which was employed Bhattacharya Distance method with a threshold at 30%. Thus was obtained the land use map that was analyzed the spatial distribution of different types of the use that is occurring in the city, identifying areas that are being used incorrectly and the main types of environmental degradation. And further, were applied the methodology proposed by Beltrame (1994), Physical Diagnosis Conservationist under some adaptations for quantifying the level of degradation or conservation study area. As results, the indexes were obtained for the parameters in the proposed methodology, allowing quantitatively analyze the degradation potential of each sector. From this perspective, considering a scale of 0 to 100, sector A and sector B had value 31.20 units of risk of physical deterioration. And the C sector, has shown its value - 34.64 units degradation risk and should be considered a priority in relation to the achievement of conservation actions

Beak-trimming methods and their effect on the performance of japanese quail pullets (Coturnix japonica)

This study aimed at verifying if beak-trimming methods in Japanese quail pullets could optimize production by decreasing stress caused by cannibalism. A total number of 816 day-old Japanese quails was distributed in a completely randomized experimental design in a 2 x 3 factorial arrangement, with two beak-trimming ages (14 and 21 days of age) and three beak-trimming sizes (not trimmed, 1/3 trimmed, or 1/2 trimmed), and 4 replicates of 34 birds per replicate. Birds were submitted to the same management and feeding conditions. Weight gain, feed intake, feed conversion ratio, and mortality were evaluated. There was no significant effect of age at beak trimming on the evaluated parameters (P>0.05), as well as no significant interaction between age at beak trimming, and beak-trimming method. There was a significant effect (P<0.01) of trimming size on performance, with the best performance observed in birds not submitted to beak trimming or had 1/2 of the beak trimmed. When the beak was more aggressively trimmed (1/2), parameters were worse. According to the obtained results, it is recommended to trim 1/3 of the beaks, which can be performed either at 14 or 21 days of age.

Prognostic value of canine frozen-thawed semen parameters on in vitro sperm-oocyte interactions

Combining the data from conventional semen analysis with oocyte penetration assays should improve the assessment of the fertilizing ability of a semen sample. Thus, the objective of the present study was to evaluate the prognostic value of various semen parameters on the in vitro interactions between frozen-thawed canine sperm and homologous oocytes. Ten ejaculates from five stud dogs (two ejaculates/dog) were collected by digital manipulation. Semen samples were evaluated, extended in Tris-egg yolk-glycerol, frozen and stored in liquid nitrogen, and thawed several weeks later. Samples were evaluated for motility and sperm populations by computer-aided semen analysis (CASA), plasma membrane integrity (carboxy-fluorescein diacetate and propidium iodide), and sperm morphology (Bengal Rose). Thawed spermatozoa were also incubated with homologous oocytes for 18 h in an atmosphere of 5% CO2 and 95% air at 38 degrees C and sperm-oocyte interactions were evaluated. Simple linear regression models were calculated, with sperm parameters as independent variables and sperm-oocyte interactions as the dependent variable. There were significant associations between: percentage of oocytes bound to spermatozoa and beat cross frequency (BCF; R-2 = 63%); percentage of oocytes that interacted with spermatozoa and BCF (R-2 = 73%); and number of penetrated spermatozoa and velocity average pathway (VAP; R-2 = 64%) and velocity straight line (VSL; R-2 = 64%). Although plasma membrane integrity and sperm morphology had little prognostic value for in vitro interactions between canine frozen-thawed sperm and homologous oocytes, some motility patterns (evaluated by CASA) were predictive of in vitro sperm-oocyte interactions. (c) 2005 Elsevier B.V. All rights reserved.

Photoelastic Stress Analysis in Screwed and Cemented Implant-Supported Dentures With External Hexagon Implants

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

Interfacial concentrations of chloride and bromide in zwitterionic micelles with opposite dipoles: Experimental determination by chemical trapping and a theoretical description

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