Desarrollo y Validación de un método espectrofotométrico UV/Vis para perfiles de disolución temporal a pH fisiológicos de tabletas de Atenolol 100 mg
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Date
2024
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Universidad Nacional de Trujillo
Abstract
El presente informe de tesis tuvo como objetivo desarrollar y validar un método espectrofotométrico UV/Vis para investigar los perfiles de disolución de tabletas de atenolol 100 mg. Se realizaron ensayos en medios de disolución con pH 1,2; 4,5 y 6,8; evaluando los parámetros de linealidad, precisión, exactitud, selectividad, robustez, estabilidad y el impacto del uso de filtro. Para ello, se empleó un equipo de disolución Sotax AT7 Smart y un espectrofotómetro UV/Visible Perkin Elmer, siguiendo las pautas de la Farmacopea de EE. UU. (USP 42), la Conferencia Internacional de Armonización (ICH) y la Asociación Española de Farmacéuticos de la Industria (AEFI). Se utilizó el aparato de paletas (tipo 2), con 900 mL de medio de disolución, a 37°C ± 0,5°C, agitación de 50 rpm y tiempos de muestreo hasta 60 minutos. Las lecturas se realizaron a una longitud de onda de 274 nanómetros. Los resultados mostraron una excelente linealidad con coeficientes de correlación y determinación superiores a 0,999 en todos los medios, junto con coeficientes de variación menores al 2% en los factores de respuesta. En exactitud, los porcentajes de recuperación oscilaron entre el 95% y el 105%, y el coeficiente de variación porcentual fue inferior al 5%. Los parámetros de precisión (repetibilidad e intermedia), robustez y el impacto del uso de filtro también demostraron una variación porcentual inferior al 2%. La selectividad presentó interferencias menores al 2%, y la estabilidad de la solución muestra fue adecuada con una diferencia absoluta inferior al 2% tras 12 y 24 horas. Se concluye que el método UV/Vis validado cumple con los requisitos de linealidad, exactitud, precisión, selectividad, robustez y estabilidad, siendo adecuado para investigar perfiles de disolución de tabletas de atenolol 100 mg
ABSTRACT The present thesis report aimed to develop and validate a UV/Vis spectrophotometric method to investigate the dissolution profiles of atenolol 100 mg tablets. Tests were performed in dissolution media with pH 1.2, 4.5 and 6.8, evaluating the parameters of linearity, precision, accuracy, selectivity, robustness, stability and the impact of filter use. For this purpose, a Sotax AT7 Smart dissolution apparatus and a Perkin Elmer UV/Visible spectrophotometer were used, following the guidelines of the U.S. Pharmacopoeia (USP 42), the International Conference on Harmonization (ICH) and the Spanish Association of Industry Pharmacists (AEFI). The paddle apparatus (type 2) was used, with 900 mL of dissolution medium, at 37°C ± 0.5°C, 50 rpm agitation and sampling times up to 60 minutes. Readings were taken at a wavelength of 274 nanometers. The results showed excellent linearity with correlation and determination coefficients greater than 0.999 in all media, along with coefficients of variation less than 2% in the response factors. In accuracy, recovery percentages ranged from 95% to 105%, and the coefficient of percentage variation was less than 5%. The parameters of precision (repeatability and intermediate), robustness and the impact of filter use also showed a percentage variation of less than 2%. Selectivity showed interferences of less than 2%, and the stability of the sample solution was adequate with an absolute difference of less than 2% after 12 and 24 hours. It is concluded that the validated UV/Vis method meets the requirements of linearity, accuracy, precision, selectivity, robustness and stability, being suitable for investigating dissolution profiles of atenolol 100 mg tablets.
ABSTRACT The present thesis report aimed to develop and validate a UV/Vis spectrophotometric method to investigate the dissolution profiles of atenolol 100 mg tablets. Tests were performed in dissolution media with pH 1.2, 4.5 and 6.8, evaluating the parameters of linearity, precision, accuracy, selectivity, robustness, stability and the impact of filter use. For this purpose, a Sotax AT7 Smart dissolution apparatus and a Perkin Elmer UV/Visible spectrophotometer were used, following the guidelines of the U.S. Pharmacopoeia (USP 42), the International Conference on Harmonization (ICH) and the Spanish Association of Industry Pharmacists (AEFI). The paddle apparatus (type 2) was used, with 900 mL of dissolution medium, at 37°C ± 0.5°C, 50 rpm agitation and sampling times up to 60 minutes. Readings were taken at a wavelength of 274 nanometers. The results showed excellent linearity with correlation and determination coefficients greater than 0.999 in all media, along with coefficients of variation less than 2% in the response factors. In accuracy, recovery percentages ranged from 95% to 105%, and the coefficient of percentage variation was less than 5%. The parameters of precision (repeatability and intermediate), robustness and the impact of filter use also showed a percentage variation of less than 2%. Selectivity showed interferences of less than 2%, and the stability of the sample solution was adequate with an absolute difference of less than 2% after 12 and 24 hours. It is concluded that the validated UV/Vis method meets the requirements of linearity, accuracy, precision, selectivity, robustness and stability, being suitable for investigating dissolution profiles of atenolol 100 mg tablets.
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Keywords
Validación. Perfiles. Atenolol. Espectrofotometría