Validación de un método espectrofotométrico UV/Vis para estudios de bioexención de tabletas de metronidazol 500 mg
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Date
2022
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Universidad Nacional de Trujillo
Abstract
El presente informe de prácticas pre - profesionales tuvo como finalidad validar un método espectrofotométrico UV/Vis para estudios de bioexención de tabletas de metronidazol 500 mg, por ello se determinó los siguientes parámetros: linealidad, exactitud, precisión, selectividad, interferencia de filtro, robustez y estabilidad, en cada uno de los medios de disolución (pH 1,2; 4,5 y 6,8). Para lo cual se trabajó con una muestra de 100 tabletas de metronidazol de 500mg, empleando para el ensayo el equipo de disolución Sotax AT7 Smart y el espectrofotómetro UV/Visible Orion AquaMate 8000. La validación del método se realizó según lo establecido en la Farmacopea de Estados Unidos 42, la Conferencia Internacional de Armonización y la Asociación Española de Farmacéuticos de la Industria; bajo las siguientes condiciones de trabajo: aparato de tipo 2 (paletas), 900 mL de volumen de medio, temperatura de 37°C +/- 0,5°C, velocidad de agitación de 75 rpm y un tiempo de muestreo de 30 minutos; la lectura espectrofotométrica se realizó a una longitud de onda de 278 nm para pH 1,2 y de 320 nm para pH 4,5 y 6,8. En cuanto al parámetro de linealidad del sistema y del método, se obtuvieron valores de coeficiente de correlación superiores a 0,999; valores de coeficiente de determinación superiores a 0,99; valores de coeficiente de variación porcentual de los factores respuesta inferiores a 2%; valores de texp superiores a ttabla en el test de linealidad de la pendiente; valores de texp inferiores a ttabla en el test de proporcionalidad y valores de Gexp inferiores a Gtabla en el test de Cochran, en cada uno de los medios de disolución. Referente al parámetro de exactitud, se obtuvieron promedios de los porcentajes de recuperación comprendidos en un rango de 95 a 105 %; valores de coeficiente de variación porcentual de los factores respuesta inferiores a 2% y valores de error relativo inferiores a 5 %, en cada uno de los medios de disolución. Respecto a los parámetros de precisión (repetibilidad y precisión intermedia), interferencia de filtro y robustez se obtuvieron valores de coeficiente de variación porcentual del factor respuesta nferiores a 2%, en cada uno de los medios de disolución. Referente al parámetro de selectividad, se obtuvieron valores de porcentaje de interferencia inferiores a 2%, en cada uno de los medios de disolución. Respecto al parámetro de estabilidad de la solución muestra, se obtuvieron valores de porcentajes de concentración final fuera del rango de 98 a 102% a las 12 horas, en cada uno de los medios de disolución. El método analítico evaluado cumple con los parámetros de linealidad, exactitud, precisión, selectividad, interferencia de filtro y robustez, en cada uno de los medios de disolución, por ello se da por validado el método espectrofotométrico UV/Vis para estudios de bioexención de tabletas de metronidazol 500 mg.
ABSTRACT The purpose of this pre - professional practice report was to validate a UV/Vis spectrophotometric method for bioexemption studies of metronidazole 500 mg tablets, for which the following parameters were determined: linearity, accuracy, precision, selectivity, filter interference, robustness and stability, in each of the dissolution media (pH 1.2; 4.5 and 6.8). For which we worked with a sample of 100 500mg metronidazole tablets, using the Sotax AT7 Smart dissolution equipment and the Orion AquaMate 8000 UV/Visible spectrophotometer for the test. The validation of the method was carried out in accordance with the provisions of the United States Pharmacopeia 42, the International Conference on Harmonization and the Spanish Association of Industry Pharmacists; under the following working conditions: type 2 apparatus (paddles), 900 mL of medium volume, temperature of 37°C +/- 0.5°C, stirring speed of 75 rpm and a sampling time of 30 minutes ; the spectrophotometric reading was performed at a wavelength of 278 nm for pH 1.2 and 320 nm for pH 4.5 and 6.8. Regarding the linearity parameter of the system and the method, correlation coefficient values greater than 0.999 were obtained; coefficient of determination values greater than 0.99; percentage variation coefficient values of the response factors less than 2%; texp values greater than ttable in the slope linearity test; texp values lower than ttable in the proportionality test and Gexp values lower than Gtable in the Cochran test, in each of the dissolution media. Regarding the accuracy parameter, averages of the recovery percentages included in a range of 95 to 105% were obtained; percentage variation coefficient values of the response factors less than 2% and relative error values less than 5%, in each of the dissolution media. Regarding the precision parameters (repeatability and intermediate precision), filter interference and robustness, percentage variation coefficient values of the response factor of less than 2% were obtained in each of the dissolution media. Regarding the selectivity parameter, interference percentage values of less than 2% were obtained in each of the dissolution media. Regarding the stability parameter of the sample solution, final concentration percentage values outside the range of 98 to 102% were obtained at 12 hours, in each of the dissolution media. The evaluated analytical method complies with the parameters of linearity, accuracy, precision, selectivity, filter interference and robustness, in each of the dissolution media, for this reason the UV/Vis spectrophotometric method for tablet bioexemption studies is considered validated. of metronidazole 500 mg.
ABSTRACT The purpose of this pre - professional practice report was to validate a UV/Vis spectrophotometric method for bioexemption studies of metronidazole 500 mg tablets, for which the following parameters were determined: linearity, accuracy, precision, selectivity, filter interference, robustness and stability, in each of the dissolution media (pH 1.2; 4.5 and 6.8). For which we worked with a sample of 100 500mg metronidazole tablets, using the Sotax AT7 Smart dissolution equipment and the Orion AquaMate 8000 UV/Visible spectrophotometer for the test. The validation of the method was carried out in accordance with the provisions of the United States Pharmacopeia 42, the International Conference on Harmonization and the Spanish Association of Industry Pharmacists; under the following working conditions: type 2 apparatus (paddles), 900 mL of medium volume, temperature of 37°C +/- 0.5°C, stirring speed of 75 rpm and a sampling time of 30 minutes ; the spectrophotometric reading was performed at a wavelength of 278 nm for pH 1.2 and 320 nm for pH 4.5 and 6.8. Regarding the linearity parameter of the system and the method, correlation coefficient values greater than 0.999 were obtained; coefficient of determination values greater than 0.99; percentage variation coefficient values of the response factors less than 2%; texp values greater than ttable in the slope linearity test; texp values lower than ttable in the proportionality test and Gexp values lower than Gtable in the Cochran test, in each of the dissolution media. Regarding the accuracy parameter, averages of the recovery percentages included in a range of 95 to 105% were obtained; percentage variation coefficient values of the response factors less than 2% and relative error values less than 5%, in each of the dissolution media. Regarding the precision parameters (repeatability and intermediate precision), filter interference and robustness, percentage variation coefficient values of the response factor of less than 2% were obtained in each of the dissolution media. Regarding the selectivity parameter, interference percentage values of less than 2% were obtained in each of the dissolution media. Regarding the stability parameter of the sample solution, final concentration percentage values outside the range of 98 to 102% were obtained at 12 hours, in each of the dissolution media. The evaluated analytical method complies with the parameters of linearity, accuracy, precision, selectivity, filter interference and robustness, in each of the dissolution media, for this reason the UV/Vis spectrophotometric method for tablet bioexemption studies is considered validated. of metronidazole 500 mg.
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Keywords
Validación, Espectrofotometría UV/Vis, Metronidazol.