RESUMO
A simple and rapid open-vessel focused microwave-assisted extraction (FMAE) method followed by LC analysis was developed for the determination of naproxen in suppositories. Parameters which might affect the FMAE method, such as nature and volume of the extraction solvent, temperature and extraction time were optimized. The extraction solvent consisted of methanol/sodium hydrogen carbonate (pH 8.7; 0.1 M) (50:50, v/v). Extractions were performed by reaching the target temperature of 70 degrees C in a 7 min linear ramp and then maintaining the target temperature for 3 min. Chromatographic analysis was performed on a Discovery RP-Amide C16 column (250 mm x 4.6 mm i.d., 5 microm particle size). The mobile phase consisted of acetonitrile/potassium dihydrogenphosphate (pH 3.0; 25 mM) (40:60, v/v). The complete analytical procedure was validated with regard to limit of quantification, linearity, precision and accuracy. The advantages of the proposed method in comparison to conventional methods are decreased extraction time, reduced solvent consumption and no further sample clean-up steps required before liquid chromatographic analysis.
Assuntos
Anti-Inflamatórios não Esteroides/química , Cromatografia Líquida/métodos , Indústria Farmacêutica/métodos , Micro-Ondas , Naproxeno/química , Supositórios/química , Química Farmacêutica/métodos , Cromatografia , Concentração de Íons de Hidrogênio , Indicadores e Reagentes/química , Fosfatos/química , Compostos de Potássio/química , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Solventes/química , Temperatura , Fatores de TempoRESUMO
To assess the relationship between aging and autonomic control of heart rate and blood pressure, cardiovascular reflex tests were performed in 70 healthy volunteers in the age range 25-71 years. R-R interval variation, heart rate change with deep breathing, 30/15 ratio and blood pressure response to standing appeared significantly declining with age. For each test we calculated the P0.99 and P0.01 confidence limits for individual observations. On the other hand, Valsalva ratio and the blood pressure response to sustained handgrip appeared to be unrelated to age. These results suggest that there is an age-dependent degradation of the mechanisms involved in the cardiovascular reflexes. The assessment of age-adjusted normal values improves the criteria for delineating abnormal from normal results in individual testing of autonomic function.