J. Pharm. Pharmacogn. Res., vol. 12, no. 3, pp. 539-547, May-Jun 2024.
DOI: https://doi.org/10.56499/jppres23.1846_12.3.539
Original Article
Development and validation of a UV spectrophotometric method for biowaiver studies in pyrazinamide tablets
[Desarrollo y validación de un método espectrofotométrico UV para estudios de bioexención en tabletas de pirazinamida]
Vanessa Saldaña-Bobadilla1*, Cintia P. Barreto-Villanueva1, Frizzi J. Ganoza-Gasco1, Enma Perez- Chauca2, Olga E. Caballero-Aquiño3, Ana E. Mantilla-Rodriguez3, Pedro M. Alva-Plasencia1, Maria S. Aurora-Prado4
1Departamento de Farmacotecnia, Facultad de Farmacia y Bioquímica, Universidad Nacional de Trujillo, Trujillo, 13011, Perú.
2Unidad de Posgrado en Farmacia y Bioquímica, Facultad de Farmacia y Bioquímica, Universidad Nacional de Trujillo, Trujillo, 13001, Perú.
3Departamento de Farmacología, Facultad de Farmacia y Bioquímica, Universidad Nacional de Trujillo, Trujillo, 13011, Perú.
4Faculdade de Ciências Farmacêuticas, Universidad de São Paulo, Av. Prof. Lineu Prestes 580-Cidade Universitària, Butantã, 05508-900, São Paulo, SP, Brasil.
*E-mail: vsaldanab@unitru.edu.peAbstract
Context: For regulatory reasons, a biowaiver is characterized as the substitution or exemption of bioavailability and/or bioequivalence research with in vitro dissolution tests, according to the Biopharmaceutical Classification System (BCS). These studies need validated quantification methods to give reliable results.
Aims: To develop and validate the UV spectrophotometric method for biowaiver studies in pyrazinamide tablets.
Methods: The parameters for validation, such as specificity, linearity, range, accuracy, precision, stability of the analytical solution, filter test, limits of detection, and quantification, were assessed according to the standards set by the guidelines of the International Conference on Harmonization and the United States Pharmacopeia. The dissolution operating conditions were 900 mL of dissolution media at pH 1.2, 4.5, and 6.8, with the paddle method at 75 rpm and sampling times of 5, 10, 15, 20, and 30 minutes.
Results: The wavelength of maximum absorbance was 268 nm for the three dissolution media. The method was linear in the range of 1.11112–13.3334 µg/mL (r2>0.998). The limits of detection ranged from 0.0157 to 0.0222 µg/mL, and the limits of quantification were between 0.0415 and 0.0546 µg/mL. The recovered values were between 99.4 and 103.0%. No interference from the placebo was observed. The relative standard deviation values were less than 2% for precision. For robustness, different conditions were evaluated as wavelengths, changes in concentration, and Whatman No. 40, 41, and 42 filters; they did not modify the method response. The samples were kept unchanged for a period of 24 hours at 25°C.
Conclusions: The UV spectrophotometric method was linear, accurate, specific, and precise in the concentration range studied and in the dissolution media at pH levels of 1.2, 4.5, and 6.8, being suitable for biowaiver studies in pyrazinamide tablets.
Keywords: antitubercular drugs; bioequivalence; drug dissolution; solubility; spectrophotometry.
Resumen
Contexto: Por razones regulatorias, una bioexención se caracteriza como la sustitución o exención de la investigación de biodisponibilidad y/o bioequivalencia con pruebas de disolución in vitro, según el Sistema de Clasificación Biofarmacéutica (SCB). Estos estudios necesitan métodos de cuantificación validados para dar confiabilidad a los resultados.
Objetivos: Desarrollar y validar el método espectrofotométrico UV para estudios de bioexención en tabletas de pirazinamida.
Métodos: Los parámetros de validación, tales como especificidad, linealidad, rango, exactitud, precisión, estabilidad de la solución analítica, prueba de filtro, límites de detección y cuantificación, fueron evaluados según los estándares establecidos por los lineamientos de la International Conference on Harmonisation y la Farmacopea de los Estados Unidos. Las condiciones operativas de disolución fueron: 900 mL de medios de disolución a pH 1,2; 4,5 y 6,8; con el método de paleta a 75 rpm, y tiempos de muestreo de 5, 10, 15, 20 y 30 minutos.
Resultados: La longitud de onda de máxima absorbancia fue 268 nm para los tres medios de disolución. El método fue lineal en el rango de 1,1112-13,3334 µg/mL (r2>0,998). Los límites de detección oscilaron entre 0,0157 y 0,0222 µg/mL, los límites de cuantificación estuvieron entre 0,0415 y 0,0546 µg/mL. Los valores recuperados se encontraron entre 99,4 y 103,0 %. No se observó interferencia del placebo. Los valores de desviación estándar relativa fueron inferiores al 2% para la precisión. Para la robustez se evaluaron diferentes condiciones como diferentes longitudes de onda, cambios en la concentración y los filtros Whatman No. 40, 41 y 42; no modificaron la respuesta del método. Las muestras se conservaron sin cambios durante un período de 24 horas a 25°C.
Conclusiones: El método espectrofotométrico UV fue lineal, exacto, específico y preciso en el rango de concentración estudiado y en los medios de disolución a niveles de pH de 1,2; 4,5 y 6,8 siendo adecuado para los estudios de bioexención en tabletas de pirazinamida.
Palabras Clave: bioequivalencia; fármaco disuelto; medicamentos antituberculosos; solubilidad; espectrofotometría.
Citation Format: Saldaña-Bobadilla V, Barreto-Villanueva CP, Ganoza-Gasco FJ, Perez-Chauca E, Caballero-Aquiño OE, Mantilla-Rodriguez AE, Alva-Plasencia PM, Aurora-Prado MS (2024) Development and validation of a UV spectrophotometric method for biowaiver studies in pyrazinamide tablets. J Pharm Pharmacogn Res 12(3): 539–547. https://doi.org/10.56499/jppres23.1846_12.3.539
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