Desenvolvimento de métodos para análise de medicamentos utilizando reflectância difusa e espectrofotometria
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Data
2006-09-20
Autores
Gotardo, Mara Andréia [UNESP]
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
Este trabalho propõe métodos por espectroscopia de reflectância difusa utilizando spot test para determinação de furosemida, hidroclorotiazida, propranolol e atenolol em formulações farmacêuticas e também um método espectrofotométrico no visível para determinação de metildopa em formulações farmacêuticas. Os métodos reflectométricos foram baseados em reações em papel de filtro, utilizando p-dimetilaminocinamaldeído (PDAC) como reagente cromogênico para furosemida e hidroclorotiazida; 2,6- dicloroquinona-4-cloroimida (DCQ) para propranolol e p-cloranil para atenolol. Estas reações produziram compostos coloridos com máximo de AR (log 1/R) em 585 nm para furosemida e hidroclorotiazida; 500 nm para propranolol e 550 nm para atenolol. Planejamentos experimentais foram empregados no desenvolvimento de todos os métodos e, as condições otimizadas para as respectivas reações de spot test foram: 10 μL de solução de furosemida em acetona, 20 μL de HCl 6,3% (m/v) em metanol e 20 μL de PDAC 0,4% (m/v) em metanol, nesta ordem, com aquecimento a 80ºC por 5 minutos; 20 μL de solução de hidroclorotiazida em acetona, 20 μL de HCl 10% (m/v) em metanol e; 20 μL de PDAC 0,4% (m/v) em metanol, nesta ordem, com aquecimento a 80ºC por 8 minutos; 30 μL de solução de propranolol em etanol 35% (v/v) e 30 μL de solução de DCQ 70 mg/mL em acetona e; 20 μL de solução de atenolol em metanol e 20 μL de p-cloranil 8,00 × 10-2 mol L-1 em dioxano. As curvas analíticas foram lineares nas faixas de concentração de 7,56 × 10-3 – 6,05 × 10-2 mol L-1 (r=0,9987) para furosemida, 3,36 × 10-2 – 1,01 × 10-1 mol L-1 (r=0,9979) para hidroclorotiazida, 1,35 × 10-2 – 8,45 × 10-2 mol L-1 (r=0.9991) para propranolol e 1,13 × 10-2 – 7,88 × 10-2 mol L-1 (r=0,9992) para atenolol. O método espectrofotométrico para a determinação de metildopa em formulações...
This work proposes methods by diffuse reflectance spectroscopy using spot tests for the determination of furosemide, hydrochlorothiazide, propranolol and atenolol in pharmaceutical formulations and also a visible spectrophotometric method for the determination of methyldopa in pharmaceutical formulations. The reflectometric methods were based on spot test reactions on filter paper, using p-dimetylaminocinnamaldehyde (p-DAC) as chromogenic reagent for furosemide and hydrochlorothiazide, 2,6-dichloroquinone -4- chloroimide (DCQ) for propranolol and, p-chloranil for atenolol. These reactions produced colored compounds with maximum AR (log 1/R) at 585 nm for furosemida and hydrochlorothiazide; 500 nm for propranolol and 550 nm for atenolol. Experimental designs were employed in the development of all methods and, the conditions optimized for the respective spot test reactions were: 10 æL of furosemide solution in acetone, 20 æL of HCl 6.3% (w/v) in methanol and 20 æL of PDAC 0.4% (w/v) in methanol, in this order, with heating at 80ºC for 5 minutes; 20 æL of hydrochlorotiazide solution in acetone, 20 æL of HCl 10% (w/v) in methanol and 20 æL of p-DAC 0.4% (w/v) in methanol, in this order, with heating at 80ºC for 8 minutes; 30 æL of propranolol solution in ethanol 35% (v/v) and 30 æL of DCQ solution at 70 mg/mL in acetone and, 20 æL of atenolol solution in methanol and 20 æL of p-cloranil at 8.00 OE 10-2 mol L-1 in dioxane. The analytical curves were linear in the concentration ranges of 7.56 OE 10-3 - 6.05 OE 10-2 mol L-1 (r=0.9987) for furosemide, 3.36 OE 10-2 - 1.01 OE 10-1 mol L-1 (r=0.9979) for hydrochlorothiazide, 1.35 OE 10-2 - 8.45 OE 10-2 mol L-1 (r=0.9991) for propranolol and (r=0.9992) for atenolol. The spectrophotometric method for the determination of methyldopa in pharmaceutical formulations used p-chloranil as chromogenic reagent and H2O2 as accelerator of the reaction.
This work proposes methods by diffuse reflectance spectroscopy using spot tests for the determination of furosemide, hydrochlorothiazide, propranolol and atenolol in pharmaceutical formulations and also a visible spectrophotometric method for the determination of methyldopa in pharmaceutical formulations. The reflectometric methods were based on spot test reactions on filter paper, using p-dimetylaminocinnamaldehyde (p-DAC) as chromogenic reagent for furosemide and hydrochlorothiazide, 2,6-dichloroquinone -4- chloroimide (DCQ) for propranolol and, p-chloranil for atenolol. These reactions produced colored compounds with maximum AR (log 1/R) at 585 nm for furosemida and hydrochlorothiazide; 500 nm for propranolol and 550 nm for atenolol. Experimental designs were employed in the development of all methods and, the conditions optimized for the respective spot test reactions were: 10 æL of furosemide solution in acetone, 20 æL of HCl 6.3% (w/v) in methanol and 20 æL of PDAC 0.4% (w/v) in methanol, in this order, with heating at 80ºC for 5 minutes; 20 æL of hydrochlorotiazide solution in acetone, 20 æL of HCl 10% (w/v) in methanol and 20 æL of p-DAC 0.4% (w/v) in methanol, in this order, with heating at 80ºC for 8 minutes; 30 æL of propranolol solution in ethanol 35% (v/v) and 30 æL of DCQ solution at 70 mg/mL in acetone and, 20 æL of atenolol solution in methanol and 20 æL of p-cloranil at 8.00 OE 10-2 mol L-1 in dioxane. The analytical curves were linear in the concentration ranges of 7.56 OE 10-3 - 6.05 OE 10-2 mol L-1 (r=0.9987) for furosemide, 3.36 OE 10-2 - 1.01 OE 10-1 mol L-1 (r=0.9979) for hydrochlorothiazide, 1.35 OE 10-2 - 8.45 OE 10-2 mol L-1 (r=0.9991) for propranolol and (r=0.9992) for atenolol. The spectrophotometric method for the determination of methyldopa in pharmaceutical formulations used p-chloranil as chromogenic reagent and H2O2 as accelerator of the reaction.
Descrição
Palavras-chave
Medicamentos - Formas farmaceuticas, Espectrofotometria, Furosemida, Formulações farmacêuticas, Spectrophotometric method, Pharmaceutical formulations, Spot tests
Como citar
GOTARDO, Mara Andréia. Desenvolvimento de métodos para análise de medicamentos utilizando reflectância difusa e espectrofotometria. 2006. 173 f. Tese (doutorado) - Universidade Estadual Paulista, Instituto de Química, 2006.