Validación de un método espectrofotométrico para cuantificar tabletas de diclofenaco sódico 50 mg en pH 6,8
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2024
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Universidad Nacional de Trujillo
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El objetivo de esta investigación fue validar un método espectrofotométrico para cuantificar diclofenaco sódico 50 mg tabletas en pH 6,8 según las normas oficiales, para lo cual se determinaron los parámetros, que incluyeron: linealidad, exactitud, precisión, estabilidad, especificidad, interferencia de filtro, robustez, límite de detección y cuantificación siguiendo los estándares establecidos de la ICH Q2 y USP NF 2023. Se trabajó con tabletas de diclofenaco sódico 50 mg, las condiciones de disolución fueron de 900 mL de medio pH 6,8; 75 rpm utilizando el método de paleta, con tiempos de muestreo de 15, 20, 30, 45, 60 y 90 minutos a una temperatura de 37°C ± 0,5°C. Las lecturas espectrofotométricas se realizaron a una longitud de onda de 276 nm. La linealidad del sistema y del método tuvieron coeficiente de determinación y correlación > 0,98; los coeficientes de variación < 2%. Los porcentajes de recuperación obtenidos oscilaron entre 95 y 105%, así mismo, los límites de cuantificación y detección se encontraron dentro de lo establecido. Para la estabilidad, las muestras se mantuvieron sin cambios durante un periodo de 6 horas en refrigeración (2°C a 8°C). Los coeficientes de variación fueron < 2% para la precisión, la diferencia absoluta en interferencia de filtro (N° 41) y robustez fue < 2%. Se concluye que, el método validado es preciso, lineal, específico y exacto, cumpliendo con los criterios de aceptación estipulados en las directrices establecidas, demostrando que es un método aplicable para evaluar perfiles de disolución de diclofenaco sódico en medio pH 6,8.
ABSTRACT The objective of this research was to validate a spectrophotometric method to quantify diclofenac sodium 50 mg tablets at pH 6.8 according to official standards, for which the parameters were determined, including: linearity, accuracy, precision, stability, specificity, filter interference, robustness, detection and quantification limit following the established standards of ICH Q2 and USP NF 2023. We worked with diclofenac sodium 50 mg tablets, the dissolution conditions were 900 mL of pH 6.8 medium; 75 rpm using the paddle method, with sampling times of 15, 20, 30, 45, 60 and 90 minutes at a temperature of 37 ° C ± 0.5 ° C. Spectrophotometric readings were taken at a wavelength of 276 nm. The linearity of the system and the method had a coefficient of determination and titration > 0.98; The coefficients of variation were < 2%. The recovery percentages obtained ranged between 95 and 105%, and the quantification and detection limits were within the established limits. For stability, the samples were kept unchanged for a period of 6 hours in refrigeration (2°C a 8°C). The coefficients of variation were < 2% for precision, the absolute difference in filter interference (No. 41) and robustness was < 2%. It is concluded that the validated method is precise, linear, specific and accurate, meeting the acceptance criteria stipulated in the established guidelines, demonstrating that it is an applicable method to evaluate dissolution profiles of sodium diclofenac in a pH 6.8 medium.
ABSTRACT The objective of this research was to validate a spectrophotometric method to quantify diclofenac sodium 50 mg tablets at pH 6.8 according to official standards, for which the parameters were determined, including: linearity, accuracy, precision, stability, specificity, filter interference, robustness, detection and quantification limit following the established standards of ICH Q2 and USP NF 2023. We worked with diclofenac sodium 50 mg tablets, the dissolution conditions were 900 mL of pH 6.8 medium; 75 rpm using the paddle method, with sampling times of 15, 20, 30, 45, 60 and 90 minutes at a temperature of 37 ° C ± 0.5 ° C. Spectrophotometric readings were taken at a wavelength of 276 nm. The linearity of the system and the method had a coefficient of determination and titration > 0.98; The coefficients of variation were < 2%. The recovery percentages obtained ranged between 95 and 105%, and the quantification and detection limits were within the established limits. For stability, the samples were kept unchanged for a period of 6 hours in refrigeration (2°C a 8°C). The coefficients of variation were < 2% for precision, the absolute difference in filter interference (No. 41) and robustness was < 2%. It is concluded that the validated method is precise, linear, specific and accurate, meeting the acceptance criteria stipulated in the established guidelines, demonstrating that it is an applicable method to evaluate dissolution profiles of sodium diclofenac in a pH 6.8 medium.
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Espectrofotometría. Diclofenaco. Solubilidad. Bioequivalencia. Equivalencia terapéutica. Validación