RESUMO
In this work, Amberlite XAD-1180 resin is used for on-line surfactant-mediated pre-concentration of sildenafil as a prior step for its fluorescent detection. In order to activate the column for sildenafil pre-concentration, the cationic surfactant (hexadecyltrimethylammoniunm bromide, HTAB) is adsorbed onto the resin. In these conditions, sildenafil is retained by HTAB-resin and then it is eluted with ethanol and analyzed by spectrofluorimetry. Drug-surfactant association produces a considerable fluorescence enhancement, increasing considerably the sensitivity of detection. Therefore, sildenafil can be pre-concentrated and quantitatively determined, with a detection limit of 0.2 ng mL(-1). The proposed method was successfully applied to the analysis of bulk drug, human urine, tablets, and local herbal medicine. Validation processes were performed by recovering studies and statistical analysis with satisfactory results.
Assuntos
Compostos de Cetrimônio/química , Piperazinas/urina , Preparações de Plantas/química , Sulfonas/urina , Tensoativos/química , Comprimidos/química , Vasodilatadores/urina , Adsorção , Cetrimônio , Fluorescência , Humanos , Limite de Detecção , Masculino , Purinas/urina , Resinas Sintéticas/química , Citrato de Sildenafila , Extração em Fase Sólida , Espectrometria de FluorescênciaRESUMO
A novel flow injection (FI)-spectrofluorimetric methodology for the determination of carvedilol in microheterogeneous medium has been developed. In the sodium dodecyl sulfate (SDS) surfactant medium, an additional fluorescence enhancement was produced by the electrolyte NaCl. A total enhancement of 3.1-fold in the native fluorescent response was achieved respect to aqueous medium. Using an excitation and emission wavelength of 286 and 341 nm, respectively, a good linear relationship was obtained in the range of 9x10(-8) to 1x10(-6) mol L(-1) with a detection limit of 3.63x10(-9) mol L(-1) (S/N=3). This method was applied to determine carvedilol in commercial pharmaceutical formulations. Good concordance was found between the nominal (6.25, 12.5 and 25.0 mg) and experimental values. The new methodology developed showed high selectivity respect to the common excipients used in pharmaceuticals. The sampling rate was 30 samples h(-1). From the fluorescent properties, binding constant for carvedilol-SDS determined was 3.2x10(2) L mol(-1).
Assuntos
Carbazóis/análise , Carbazóis/química , Análise de Injeção de Fluxo/métodos , Micelas , Propanolaminas/análise , Propanolaminas/química , Espectrometria de Fluorescência/métodos , Métodos Analíticos de Preparação de Amostras , Carvedilol , Eletrólitos/química , Fluorescência , Concentração de Íons de Hidrogênio , Modelos Lineares , Concentração Osmolar , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Dodecilsulfato de Sódio/química , Tensoativos/química , Fatores de TempoRESUMO
A simple FI-fluorimetric analytical methodology for the continuous and sequential determination of rhodamine B (RhB) in cosmetic products has been developed and evaluated in terms of sensibility and selectivity. The influence of several surfactant solutions on RhB fluorescence signal has been studied; particular attention was paid in the aggregation behavior of RhB-SDS system. Linear response has been obtained in the range of 1.6 x 10(-9) and 1 x 10(-6) mol L(-1), with a detection limit of 5 x 10(-10) mol L(-1). The novel technique provides a simple dissolution of sample, on-line filtration with sampling rate higher than 100 samples h(-1) and has been satisfactorily applied to the RhB determination in commercial lipsticks.
RESUMO
A new sensitive and selective preconcentration-fluorimetric method for determination of terazosin based on its native fluorescence was developed. The analyte, initially present in aqueous matrix, was treated with an extractive non-ionic surfactant solution and separated by the clouding phenomenon. The optimum analytical conditions for terazosin assay were established. Under these conditions, linear calibration curves were obtained over the range of 1x10(-5) to 7.0 microg mL(-1) with detection and quantification limits of 1.11x10(-5) and 3.7x10(-5)microg mL(-1), respectively. Additionally, the binding constant (K(B)) for the terazosin-PONPE 7.5 system was determined given a value of 1028 L mol(-1). The developed coupled methodology, which thoroughly satisfies the typical requirements for pharmaceutical control processes, was proved to be appropriate for monitoring terazosin in actual pharmaceutical formulations and biological fluid sample. The results were validated by recovery test and by comparison with other reported methods, being highly satisfactory.