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.

A stability-indicating LC method for difloxacin in the presence of degradation products

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

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)

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)

Proposta de controlador de carga com MPPT utilizando LabVIEW

This paper presents one proposal of the energy management's model system using photovoltaic panels. The module proposed seeks to monitor photovoltaic panels, which have intermittency in power generation caused by environmental or load conditions, in order to control the coupling between the panel and the load - through the charge controller, of aiming that the panel's operation will be always on the maximum power transfer point as possible. For this, it used the maximum power point tracking technique - MPPT, implemented in LabVIEW software, also utilizing the data acquisition card NI myDAQ. In addition, it was implemented the controller access remote module, from the sharing of network data, so the panels performance can be through a tablet, monitored and controlled with no need for direct contact with the Supervisory server

Proposta de controlador de carga com MPPT utilizando LabVIEW

This paper presents one proposal of the energy management's model system using photovoltaic panels. The module proposed seeks to monitor photovoltaic panels, which have intermittency in power generation caused by environmental or load conditions, in order to control the coupling between the panel and the load - through the charge controller, of aiming that the panel's operation will be always on the maximum power transfer point as possible. For this, it used the maximum power point tracking technique - MPPT, implemented in LabVIEW software, also utilizing the data acquisition card NI myDAQ. In addition, it was implemented the controller access remote module, from the sharing of network data, so the panels performance can be through a tablet, monitored and controlled with no need for direct contact with the Supervisory server

Turbidimetric Spectroscopy for the Evaluation of Metalworking Fluids Stability

The stability of oil-in-water (O/W) emulsions used as metalworking fluids is a key factor for the economical and environmental balance of the entire metalworking process because used and broken fluids must be recycled or disposed. In this study, the ability of turbidimetric spectroscopy in the ultraviolet and visible light range to detect metalworking fluids destabilization was evaluated. Destabilization was achieved by adding calcium chloride, thus achieving accelerated aging, which leads to coalescence, creaming, and complete emulsion separation. The stability of the metalworking fluids at 5% volumetric concentration in deionized water was monitored using a spectroscopic turbidimeter composed of an optical probe for in-line measurements. Destabilization was also monitored by measuring the vertical profile of backscattered and transmitted light. The results of this offline measurement system were compared with those from the in-line spectroscopic sensor, indicating that the latter can provide local, real-time information on emulsion destabilization, thus enabling control actions.

Stability-indicating methods for the enantioselective determination of dihydropyridines by high performance liquid chromatography and capillary electrophoresis

This paper presents simple, rapid, precise and accurate stability-indicating HPLC and CE methods, which were developed and validated for the determination of nitrendipine, nimodipine and nisoldipine. These drugs are calcium channel antagonists of the 1,4-dihydropyridine type which are used in the treatment of cardiovascular diseases. Experimental results showed a good linear correlation between the area and the concentration of drugs covering a relatively large domain of concentration in all cases. The linearity of the analytical procedures was in the range of 2.0-120.0 mu g mL-1 for nitrendipine, 1.0-100.0 mu g mL(-1) for nimodipine and 100.0-600.0 mu g mL(-1) for nisoldipine, the regression determination coefficient being higher than 0.99 in all cases. The proposed methods were found to have good precision and accuracy. The chemical stability of these drugs was determined under various conditions and the methods have shown adequate separation for their enantiomers and degradation products. In addition, degradation products produced as a result of stress studies did not interfere with the detection of the drugs' enantiomers and the assays can thus be considered stability-indicating.

PRODUÇÃO DE BIOMASSA E COMPOSIÇÃO QUÍMICA DE ADUBOS VERDES CULTIVADOS NO VALE DO RIBEIRA

A contribuição da adubação verde com leguminosas para melhoria do solo e produção agrícola depende em primeiro lugar da produção de biomassa e da sua composição química, que variam em função da espécie, região e estação de cultivo. Objetivo do presente trabalho foi avaliar a composição química da biomassa produzida por adubos verdes no Vale do Ribeira, São Paulo, Brasil. Para tal, foi conduzido um experimento em Pariquera-Açu-SP, no ano agrícola 2006/2007, em blocos casualizados, com quatro tratamentos (três adubos verdes e vegetação espontânea) e cinco repetições. Aos 30, 60, 90 e 120 dias após a semeadura, foram coletadas amostras em 1 m² da parte aérea das plantas e determinada a matéria fresca e seca, bem como a composição da biomassa. Crotalária, guandu e mucuna produziram, em ordem decrescente, as maiores quantidades de biomassa e foram mais eficientes do que a vegetação espontânea. A biomassa produzida pelos adubos verdes apresentou qualidade superior à produzida pela vegetação espontânea. Crotalária e guandu apresentam maior proporção de matéria seca acumulada no caule que possui baixo teor de N, alta relação C/N e L/N, variáveis que tornam a decomposição dos resíduos mais lenta. A análise particionada da matéria seca permite indicação mais precisa da composição química dos resíduos e a previsão da disponibilidade dos nutrientes no solo.