Determination of cadmium in river water samples by flame AAS after on-line preconcentration in mini-column packed with 2-aminothiazole-modified silica gel

A rapid and sensitive method was developed to determine trace levels of Cd2+ ions in an aqueous medium by flame atomic absorption spectrometry, using on-line preconcentration in a mini-column packed with 100 mg of 2-aminothiazol modified silica gel (SiAT). The Cd2+ ions were sorbed at pH 5.0. The preconcentrated Cd2+ ions were directly eluted from the column to the spectrometer's nebulizer-burner system using 100 μL of 2 mol L-1 hydrochloric acid. A retention efficiency of over 95% was achieved. The enrichment factor (calculated as the ratio of slopes of the calibration graphs) obtained with preconcentrations in a mini-column packed with SiAT (A = -1.3 × 10-3 + 1.8 × 10-3 [Cd2+]) and without preconcentrations (A = 4 × 10-5 + 3.5 × 10-3[Cd2+]), was 51 and the detection limit calculated was 0.38 μg L-1. The preconcentration procedure was applied to determine trace levels of Cd in river water samples. The optimum preconcentration conditions are discussed herein.

Determination of Cu, Ni and Pb in Aqueous Medium by FAAS after Pre-Concentration on 2-Aminothiazole Modified Silica Gel

This work describes the synthesis and characterization of 2-aminothiazole modified silica gel (SiAT), and the results of a study of the adsorption and pre-concentration (in batch and using a flow-injection system coupled to an absorption atomic spectrometer) of Cu(II), Ni(II) and Pb(II) in aqueous medium. The adsorption capacities for each metal ions in mmol g -1 were: Cu(II)= 1.18, Ni(II)= 1.15 and Pb(II)= 1.10. The results obtained in the flow experiments showed a recovery of practically 100% of the metal ions adsorbed in a mini-column packed with 100 mg of SiAT, using 100 μL of 2.0 mol L -1 HCl solution as eluent. The sorption-desorption of the metal ions made possible the application of a flow-injection system for the pre-concentration and quantification by FAAS of metal ions at trace level in natural water samples digested and not digest by an oxidizing UV photolysis.

Determination of calcium by atomic absorption spectrophotometry applied to the preparation of alginate:chitosan complexes

Polysaccharicles, as alginate and chitosan, have been used to obtain modified release dosage forms. Alginate, due to its property of building gels during the complex formation with calcium ions, allows the building of capsules containing a core constituted by calcium alginate. This work had for objective to determine the appropriate calcium concentration for the preparation of alginate-chitosan capsules, by means of calcium quantification using atomic absorption spectrophotometry. The methodology of calcium quantification was validated through analysis of the limit of detection, precision, accuracy and recovery of the method. The capsules, containing or not the drug, were prepared by the complex coacervation/ionotropic gelification method. Calcium was quantified after samples mineralization and dilution in lantanium solution. The results showed that the amount of calcium incorporated into the capsules depends on the amount of calcium added to the medium, and this ratio increases until the concentration of 1.5% of initial calcium chloride and above this concentration there is a decrease in the proportion of calcium bonded. It was observed that the proportion of calcium that links to the polymer is inversely proportional to the amount of calcium added. The calcium amount incorporated depends on the concentration of the polymeric dispersions used as well as on the ratio between the two polymers.

Development and validation of an UV spectrophotometric method for determination of gatifloxacin in tablets

A simple, sensitive and accurate spectrophotometric method was developed for the assay of gatifloxacin in raw material and tablets. Validation of the method yielded good results concerning range, linearity, precision and accuracy. The absorbance was measured at 287 nm for gatifloxacin tablet solutions. The linearity range was found to be 4.0-14.0 μg/mL for gatifloxacin. It was also found that the excipients in the commercial tablets did not interfere with the method.

Validation of UV spectrophotometric method for determination of lomefloxacin in pharmaceutical dosage form

A simple and reproducible method was developed for the assay of lomefloxacin in tablets. The excipients in the commercial tablet preparation did not interfere with the assay. Beer's law is obeyed in the range 2.0-9.0 μg.mL-1 at λmax 280 nm. The molar absorptivity was calculated. Six triplicate analyses of solutions containing six different concentrations of the examined drug were carried out and gave a mean correlation coefficient 0.9997. The proposed method was applied to the determination of the examined drug in coated tablet and the results demonstrated that the method is equally accurate, precise and reproducible as the official methods.

Polymer light emitting devices with Langmuir Blodgett (LB) films of a polyfluorene derivative

Polyfluorenes are promising materials for the emitting layer of polymer light emitting devices (PLEDs) with blue emission. In this work, we report on PLEDs fabricated with Langmuir-Blodgett (LB) films of a polyfluorene derivative, namely poly(9,9-di-hexylfluorenediyl vinylene-alt-1,4-phenylenevinylene) (PDHF-PV). Y-type LB films were transferred onto ITO substrates at a surface pressure of 35 mN m-1 and with dipping speed of 3 mm min -1. A thin aluminum layer was evaporated on top of the LB film, thus yielding a sandwich structure (ITO/PDHF-PV(LB)/Al). Current-voltage (I vs V) measurements indicate that the device displays a classical behavior of a rectifying diode. The threshold value is approximately 5 V, and the onset for visible light emission occurs at ca. 10 V. From the a.c. electrical responses we infer that the active layer has a typical behavior of PLEDs where the real component of ac conductivity obeys a power-law with the frequency. Cole-Cole plots (Im(Z) vs. Re(Z)) for the device exhibit a series of semicircles, the diameter of which decreases with increasing forward bias. This PLED structure is modeled by a parallel resistance and capacitance combination, representing the dominant mechanisms of charge transport and polarization in the organic layer, in series with a resistance representing the ITO contact. Overall, the results presented here demonstrate the feasibility of LEDs made with LB films of PDHF-PV.

A new antifungal phenolic glycoside derivative and iridoids and lignans from Alibertia sessilis (Vell.) K. Schum. (Rubiaceae)

A new antifungal phenolic glycoside, 3,4,5-trimethoxyphenyl-1-O-β-D- (5-O-syringoyl)-apiofuranosyl-(1→6)-β-D-glucopyranoside (1), together with four known iridoids, geniposidic acid (2), geniposide (3), 6α-hydroxygeniposide (4) and 6β-hydroxygeniposide (5); two lignans, (+)-lyoniresinol-3α-O-β-D-glucopyranoside (6), (-)-lyoniresinol- 3α-O-β-D-glucopyranoside (7); and two phenolic acids, chlorogenic (8) and salicylic acids (9) and D-manitol (10), were isolated from the ethanolic extract of the stems of Alibertia sessilis. Structures of 1 and of the known compounds were determined by spectroscopic analysis. All compounds isolated were evaluated for their antifungal activities against two phytopathogenic fungi strains Cladosporium cladosporioides and C. sphaerospermum by direct bioautography. ©2007 Sociedade Brasileira de Química.

Gravitational field of a straight cosmic string in the framework of higher-derivative gravity

The gravitational properties of a straight cosmic string are studied in the linear approximation of higher-derivative gravity. These properties are shown to be very different from those found using linearized Einstein gravity: there exists a short range gravitational (anti-gravitational) force in the nonrelativistic limit; in addition, the deflection angle of a light ray moving in a plane orthogonal to the string depends on the impact parameter. © 2008 World Scientific Publishing Company.

Determination of calcium and magnesium in hydroethanolic extracts of propolis by atomic absorption flame spectrophotometry

Propolis is a natural product collected by honeybees and has a large range of pharmacological activity, including antimicrobial, antitumoral, antioxidant and anti-inflammatory. Its use as a popular medicine is increasing all over the world, creating a need for quality control of the commercial products. In this study the levels of calcium and magnesium in commercial hydroalcoholic propolis extracts from varies states of Brazil were determined by atomic absorption flame spectrophotometry and different values were obtained for northern and southern states. This study can be extended to the analysis of metals that are harmful to health. The results showed that the calibration curves were linear over a wide concentration range (0.5-4.0 μg.mL -1 for calcium and 0.05-0.4 μg.mL -1 for magnesium) with good correlation coefficients (0.999 and 0.988, respectively). Good analytical recovery (94%) was obtained. The proposed method showed adequate precision and relative standard deviation lower than 2 %. The method is accurate and precise as well as having advantages such as simplicity and speed.

Estudo de metodologia analítica para a determinação do cetoconazol em formulações farmacêuticas

Ketoconazole is a synthetic broad-spectrum oral and topical antifungal drug derived from imidazole, effective in the treatment of superficial mycoses and systemic infections. In this study we have tested several methods to analyze ketoconazole in various pharmaceutical products containing this drug, employing techniques such as UV and IR spectrophotometry and thermal analysis. The results showed that UV spectrophotometry is a fast, practical and economical method and indicated that other methods, such as IR spectrophotometry and thermal analysis, could be good alternative methods for ketoconazole analysis in certain pharmaceutical forms.

Evaluation of hardness and colour change of soft liners after accelerated ageing.

INTRODUCTION: Soft liners have been developed to offer comfort to denture wearers. However, this comfort is compromised when there is a change in the properties of the material, causing colour change, solubility, absorption and hardening. These characteristics can compromise the longevity of soft liners. AIM: The aim of this in vitro study was to investigate the effect of ageing on both the hardness and colour change of two soft liners following accelerated ageing. METHODS: Two denture liners, one resin based (Trusoft, Bosworth, Illinois, USA) and one silicone based (Ufi Gel P, Voco GMBH, Cuxhaven, Germany), were tested in this study for both hardness (using the Shore A scale) and colour change (using the CIE L*a*b* colour scale), initially and after 1008 hours (6 weeks) of accelerated ageing. Statistical analysis was performed using the unpaired t-test with the Welch correction. RESULTS: These indicated that both materials increased in hardness and underwent colour change after accelerated ageing. The initial hardness of Trusoft was far lower than that of Ufi Gel P (18.2 Shore A units vs 34.8 Shore A units). However, for Trusoft the changes for both hardness (from 18.2 to 52.1 Shore A units) and colour change (16.85 on the CIE L*a*b* colour scale) were greater than those for Ufi Gel P, for which hardness changed from 34.8 to 36.5 Shore A units and the colour change was 5.19 on the CIE L*a*b* colour scale. CONCLUSIONS: Ufi Gel P underwent less hardness and colour change after accelerated ageing than Trusoft. On the other hand, the use of Trusoft may be preferable in cases where initial softness is a major consideration, such as when relining an immediate denture after implant surgery.

Color alteration of the paint used for iris painting in ocular prostheses

The purpose of this study was to assess color alteration of the paints used for iris painting in artificial eyes. Five disks of heat cured acrylic resin were confectioned by microwave energy for each paint analyzed, in a total of 40 specimens. Each specimen consisted of a colorless acrylic resin disk and another of equal size, of scleral white colored acrylic resin, with the painting interposed between the two disks. The specimens were submitted to an accelerated aging process in a chamber under ultraviolet radiation for 1,008 hours. To assess color variation, a reflective spectrophotometer was used. The results were statistically analyzed by ANOVA and the Tukey test (p < 0.05). All the paints underwent chromatic alteration. The oil paint presented the highest resistance to accelerated aging.

LMI-based digital redesign of linear time-invariant systems with state-derivative feedback

A simple method for designing a digital state-derivative feedback gain and a feedforward gain such that the control law is equivalent to a known and adequate state feedback and feedforward control law of a digital redesigned system is presented. It is assumed that the plant is a linear controllable, time-invariant, Single-Input (SI) or Multiple-Input (MI) system. This procedure allows the use of well-known continuous-time state feedback design methods to directly design discrete-time state-derivative feedback control systems. The state-derivative feedback can be useful, for instance, in the vibration control of mechanical systems, where the main sensors are accelerometers. One example considering the digital redesign with state-derivative feedback of a helicopter illustrates the proposed method. © 2009 IEEE.

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

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)