Optimisation of a sample preparation method for the determination of fumonisin B-1 in rice

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Development of a method for sampling and determination of corrosion inhibitors in modified atmospheres

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Development of a simple method for determination of NO2 in air using digital scanner images

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Development and validation of an economic, environmental friendly and stability-indicating analytical method for determination of ampicillin sodium for injection by RP-HPLC

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

Validation of a stability indicating capillary electrophoresis method for the determination of darunavir in tablets and comparison with the of infrared absorption spectroscopic method

Darunavir (DRV) is a protease inhibitor used in the treatment of HIV infection, which constitutes a keystone in the therapy of patients infected with this virus. There is no monograph described in official compendia. The literature provides few methods of analysis for the determination of DRV in pharmaceuticals which include TLC, IR, UPLC, HPLC, HPLC-MS, HPLC-MS/MS, but there are no reports of the use of capillary electrophoresis (CE) for the determination of this drug. Thus, this research proposed the development and validation of a CE method for the determination of DRV in tablets. The method was completely validated according to the International Conference on Harmonization guidelines, showing linearity, selectivity, precision, accuracy and robustness. The migration was achieved in less than 1 minute using fused-silica uncoated capillary with an id of 50 μm and total length of 21 cm and voltage of +20 kV. The sample injection was performed in the hydrodynamic mode. The method was linear over the concentration range of 50-200 μg mL-1 with correlation coefficient 0.9998 and limits of detection and quantification of 7.29 and 22.09 μg mL-1, respectively. The drug was subjected to acid, base, oxidation and photolysis degradation. Degradation products were found interfering with the assay of DRV, therefore the method can be regarded as stability indicating. The validated method is useful and appropriate for the routine quality control of DRV in tablets.

Validation of a stability-indicating HPLC method with diode array detection for the determination of beclomethasone dipropionate in aqueous suspension for nebulizer

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A first-derivative spectrophotometric method for the determination of ciprofloxacin hydrochloride in ophthalmic solution

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Development and validation of infrared spectroscopy method for the determination of darunavir in tabets

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Validation of a HPLC method for determination of glutamine in food additives using post-column derivatization

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Direct determination of Cu, Cd, Ni and Pb in aquatic humic substances by graphite furnace atomic absorption spectrometry

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

Voltammetric determination of L-dopa using an electrode modified with trinuclear ruthenium ammine complex (Ru-red) supported on Y-type zeolite

The L-dopa is the immediate precursor of the neurotransmitter dopamine. Unlike dopamine, L-dopa easily enters the central nervous system and is used in the treatment of Parkinson's disease. A sensitive and selective method is presented for the voltammetric determination of L-dopa in pharmaceutical formulations using a carbon paste electrode modified with trinuclear ruthenium ammine complex [(NH3)(5)Ru-III-O-Ru-IV(NH3)(4)-O-Ru-III(NH3)(5)](6+) (Ru-red) incorporated in NaY zeolite. The parameters which influence on the electrode response (paste composition, potential scan rate, pH and interference) were also investigated. The optimum conditions were found to an electrode composition (m/m) of 25% zeolite containing 6.7% Ru, 50% graphite and 25% mineral oil in acetate buffer at pH 4.8. Voltammetric peak currents showed a linear response for L-dopa concentration in the range between 1.2 x 10(-4) and 1.0 x 10(-2) Mol l(-1) (r = 0.9988) with a detection limit of 8.5 x 10(-5) mol l(-1). The variation coefficient for a 1.0 x 10(-3) mol l(-1) L-dopa (n = 10) was 5.5%. The results obtained for L-dopa in pharmaceutical formulations (tablet) was in agreement with compared official method. In conclusion, this study has illustrated that the proposed electrode modified with Ru-red incorporated zeolite is suitable valuable for selective measurements of L-dopa. (C) 2004 Elsevier B.V. All rights reserved.

Voltammetric determination of isoprenaline in pharmaceutical preparations using a copper(II) hexacyanoferrate(III) modified carbon paste electrode

The electroanalytical determination of isoprenaline in pharmaceutical preparations of a homemade carbon paste electrode modified with copper(II) hexacyanoferrate(III) (CuHCF) was studied by cyclic voltammetry. Several parameters were studied for the optimization of the sensor such as electrode composition, electrolytic solution, pH effect, potential scan rate and interferences in potential. The optimum conditions were found in an electrode composition (in mass) of 15% CuHCF, 60% graphite and 25% mineral oil in 0.5 mol l(-1) acetate buffer solution at pH 6.0. The analytical curve for isoprenaline was linear in the concentration range from 1.96 x 10(-4) to 1.07 x 10(-3) mol l(-1) with a detection limit of 8.0 x 10(-5) mol l(-1). The relative standard deviation was 1.2% for 1.96 x 10(-4) mol l(-1) isoprenaline solution (n=5). The procedure was successfully applied to the determination of isoprenaline in pharmaceutical preparations; the CuHCF modified carbon paste electrode gave comparable results to those results obtained using a UV spectrophotometric method. (C) 2004 Elsevier B.V. All rights reserved.

Flow-injection spectrophotometric determination of dipyrone in pharmaceutical formulations using ammonium molybdate as chromogenic reagent

A simple and rapid flow-injection spectrophotometric method is reported for the determination of dipyrone in pharmaceutical formulations. The method is based on the reaction of dipyrone with ammonium molybdate in acidic medium to produce blue molybdenum, which was detected spectrophotometrically at 620 nm. The analyte was determined in a single-line flow system. The calibration curve obtained was linear in the range of 5x10(-4) to 8x10(-3) mol L-1 for dipyrone concentration and the precision ( s r =1.7%) was satisfactory. The method proved to be selective and adequately sensitive. Application of the method to the analysis of pharmaceutical samples resulted in excellent accuracy; the percent mean recoveries were in the range 95.3%-101% and relative errors less than 5.0% for five pharmaceutical formulations were found.

Methodologies for ribeye area determination in goats

The aim of this study was to evaluate the accuracy of a number of methodologies, i.e. PLANIMETER, GEOMETRIC, GRID, UNESP-GRID, UFSM, ZEISS and DELTA-T, in determining ribeye area (REA) of 65 Saanen goats of varying body condition. Goats were grouped according to body weight at slaughter (5.3, 11.2, 12.9, 16.4, 21.0, 22.1, 27.7, 28.6 and 35.2kg). Tracing based on transverse section between the 13th thoracic and I st lumbar vertebrae was used to determinate REA. There was no significant interaction between methodologies and body weight at slaughter. PLANIMETER, UNESP-GRID, GEOMETRIC and UFSM methods were similar in average values to the standard DELTA-T method. The REA was overestimated by the GRID and underestimated by the ZEISS method. The UNESP-GRID, GEOMETRIC and UFSM methods have coincident curves comparable to DELTA-T, when used to estimate goat REA. The UNESP-GRID and GEOMETRIC were the methods of choice based on accuracy, practicality and feasibility. (c) 2005 Elsevier B.V. All rights reserved.

Poultry feed metabolizable energy determination using total or partial excreta collection methods

The aim of this work was to compare the efficiency of total (TC) or partial (PC) collection excreta methods to determine metabolizable energy in poultry feeds. A number of 180 12- to 21-day-old broilers were distributed into two treatments of six replicates of 10 birds each. A reference-diet was formulated to supply broiler requirements, and the test-diets consisted of 60% of reference diets and 40% of corn or soybean meal. Celite was added at 1% to the diets as a marker. Excreta and diet samples were analyzed for dry matter, energy, nitrogen, and acid-insoluble ash (AIA). AME of corn determined by partial collection (PC) was higher (3544 kcal/kg) as compared to total collection (TC) (3133 kcal/kg). However, no difference were observed for soybean meal (1797 vs. 1821 kcal/kg) between both methods. Marker recovery rates in the excreta were 101, 111, and 96% for the basal-diet, and the test-diets with corn or soybean meal, respectively. This result indicates the importance of marker recovery rate in the excreta to evaluate feed AME and digestibility.