Desenvolvimento de método analítico para estudo de degradação forçada de cefalotina sódica na forma farmacêutica pó liofilizado para solução injetável

Pós-graduação em Ciências Farmacêuticas - FCFAR

Effect of method of caries induction on aged resin-dentin bond of primary teeth

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

Trichomes related to an unusual method of water retention and protection of the stem apex in an arid zone perennial species

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Screening the toxicity and biodegradability of petroleum hydrocarbons by a rapid colorimetric method

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Enhanced photoelectrocatalytic degradation of an acid dye with boron-doped TiO2 nanotube anodes

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

Rapid preparation of (BiO)(2)CO3 nanosheets by microwave-assisted hydrothermal method with promising photocatalytic activity under UV-Vis light

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Thermal degradation and lifetime estimation of poly(ether imide)/carbon fiber composites

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

In situ selective determination of methylmercury in river water by diffusive gradient in thin films technique (DGT) using baker's yeast (Saccharomyces cerevisiae) immobilized in agarose gel as binding phase

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

Otimização de método para analise de tebutiurom, diurom e seus produtos de degradação em água superficial

In 2001, it was estimated that pesticide used worldwide exceeded 2.27 billion kilograms, over 35%, of which, were herbicides. Brazil is considered one of the leaders in the production of sugarcane and mainly ethanol as fuel. The monoculture of sugarcane requires the usage of a range of pesticides, among these, the herbicides diuron and tebuthiuron. The degradation products most studied (DCA and DCPU) are diuron's, especially for toxicological characteristics of this herbicide that is identified as carcinogen and suspected to be endocrine disruptor in mammals. After optimization of the chromatographic separation using HPLC-UV, the analytical curve was constructed in solvent and subsequently in the matrix (surface water). The extraction method contains the usage of SPE (solid phase extraction) (Strata-X, 200 mg/6 mL), applicating 1L of sample and elution with 5 mL of acetonitrile / methanol (50:50, v/v). Analysis by HPLC/UV was performed in gradient mode, acetonitrile/water (70/30-74/26 by 1 min, 74/26 - 78/22 till 3.2 min, returning to initial conditions and remaining this way until 10 min), 018 column (Phenomenex, 4.6 mm diameter, 250 mm long and 5pm particle size) and detection at 254 nm. Tests F and t were performed to verify the presence of the matrix effect. There was matrix effect to all analytes, ranging from -33% (DCA) and 38% (tebuthiuron). Thereby the method was optimized and validated for analysis of diuron, tebuthiuron, and DCPU DCA in surface water using HPLC/UV. The data obtained show that in order to assure the analytical reliability desired the use of the analytical curves in the matrix for the quantification of these analytes in water is required.

Development and validation of a simple, rapid and stability-indicating high performance liquid chromatography method for quantification of norfloxacin in a pharmaceutical product

A stability-indication high performance liquid chromatographic method has been developed for the determination of norfloxacin in tablet dosage forms. Optimum separation was achieved in less than 7 minutes using Eclipse Plus Zorbax C18 Agilent, 150 mm×4.6 mm i.d., 5 μm particle size column. The analyte was resolved by using a mobile phase 5% acetic acid aqueous solution and methanol (80:20, v/v) at a flow rate 1.0 ml/min on an isocratic high performance liquid chromatographic system at a wavelength of 277 nm. Linearity, system suitability, precision, sensitivity, selectivity, specific, and robustness were established by International Conference Harmonization guidelines. For stress studies the drug was subjected to photolysis, oxidation, acid, alkaline and neutral conditions. The analytical conditions and the solvent developed provided good resolution within a short analysis time and economic advantages. The proposed method not required sophisticated and expensive instrumentation.

Stability study of darunavir ethanolate tablets applying a new stability-indicating HPLC method

Chemical and physical degradation of drugs may result in altered therapeutic efficacy and even toxic effects. Therefore, the aim of this work was to study the stability of darunavir and to develop and validate a liquid chromatography (LC) method to determine darunavir in raw material and tablets in the presence of degradation products. The novel method showed to be linear from 6.0 to 21.0 μg/mL, with high precision (CV < 2%) and accuracy (recuperation of 99.64%). It is simple and reliable, free of placebo interferences. The robustness of the method was evaluated by a factorial design using seven different parameters. Forced degradation study was done under alkaline, acidic, and oxidative stress at ambient temperature and by heating. The LC method was able to quantify and separate darunavir and its degradation products. Darunavir showed to be unstable under alkaline, acid, and oxidative conditions. The novelty of this study is understanding the factors that affect darunavir ethanolate stability in tablets, which is the first step to unravel the path to know the degradation products. The novel stability-indicating method can be used to monitor the drug and the main degradation products in low concentrations in which there is linearity.

Development of an innovative, ecological and stability-indicating analytical method for semiquantitative analysis of ampicillin sodium for injection by thin layer chromatography (TLC)

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)

Unexpected toxicity decrease during photoelectrochemical degradation of atrazine with NaCl

This report shows an unexpected toxicity decrease during atrazine photoelectrodegradation in the presence of NaCl. Atrazine is a pesticide classified as endocrine disruptor occurring in industrial effluents and agricultural wastewaters. We therefore studied the effects of the degradation method, electrochemical and electrochemical photo-assisted, and of the supporting electrolyte, NaCl and Na2SO4, on the residual toxicity of treated atrazine solutions. We also studied the toxicity of treated atrazine solutions using Results show that at initial concentration of 20 mg L-1, atrazine was completely removed in up to 30 min using 10 mA cm(-2) electrolysis in NaCl medium, regardless of the electrochemical method used. The total organic carbon removal by the photo-assisted method was 82% with NaCl and 95% with Na2SO4. The solution toxicity increased during sole electrochemical treatment in NaCl, as expected. However, the toxicity unexpectedly decreased using the photo-assisted method. This finding is a major discovery because electrochemical treatment with NaCl usually leads to the formation of toxic chlorine-containing organic degradation by-products.