Validación de método analítico de valoración de Bisoprolol fumarato 2.5 mg tableta recubierta por método de cromatografía líquida de alta resolución (HPLC) - 2023
Fecha
2025
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Universidad Nacional San Luis Gonzaga
Resumen
La validación de métodos analíticos forma parte integral del sistema de control de calidad, siendo
un proceso crítico en las industrias farmacéutica, garantizar la calidad y seguridad de los
productos farmacéuticos. En este trabajo presentamos la validación de un método analítico de
valoración de Bisoprolol fumarato 2.5 mg tableta recubierta, mediante la técnica de cromatografía
líquida de alta performance establecido en la USP 2023. Entre los parámetros estadísticos usados
en la presente validación se encuentran: La linealidad; se producen resultados proporcionales a la
concentración del analito, queda demostrado por un coeficiente de correlación de r= 0.999, (valor
mínimo permisible = 0.997). La exactitud mide la cercanía de los resultados conseguidos por esta
metodología y el valor real. Empleando el test de student para demostrar la exactitud del método
analítico se obtuvo un texp (-0.097) que es menor al t de las tablas (2.306); por lo tanto, no existe
diferencia significativa entre la recuperación media y la cantidad añadida de analito, es decir que
el porcentaje de recuperación del analito es muy cercano al 100%. La precisión del método
analítico indica grado de concordancia o dispersión de resultados de la prueba. Los valores de
RSD obtenidos, (0.65% para repetibilidad y 0.93% para precisión intermedia), demuestran la
precisión del método analítico (valor máximo permitido, RSD = 2.0%). El método es específico,
como tampoco se detectó presencia de productos de degradación del Bisoprolol fumarato al
someter al principio activo a diferentes procedimientos de degradación forzada, por lo tanto, el
método es selectivo.
The validation of analytical methods is an integral part of the quality control system, being a critical process in the pharmaceutical industries to ensure the quality and safety of pharmaceutical products. In this work we present the validation of an analytical method for titration of Bisoprolol fumarate 2.5 mg coated tablet, using the high-performance liquid chromatography technique established in USP 2023. Among the statistical parameters used in the present validation are: Linearity; results are produced proportional to the concentration of the analyte, is demonstrated by a correlation coefficient of r= 0.999, (minimum permissible value = 0.997). Accuracy measures the closeness of the results achieved by this methodology and the true value. Using the student's test to demonstrate the accuracy of the analytical method, a texp (-0.097) was obtained, which is lower than the t of the tables (2.306); therefore, there is no significant difference between the average recovery and the added amount of analyte, that is to say the percentage recovery of the analyte is very close to 100%. The precision of the analytical method indicates the degree of agreement or dispersion of test results. The RSD values obtained (0.65% for repeatability and 0.93% for intermediate precision) demonstrate the precision of the analytical method (maximum allowable value, RSD = 2.0%). The method is specific, as the presence of degradation products of Bisoprolol fumarate was not detected when the active principle was subjected to different forced degradation procedures, therefore, the method is selective.
The validation of analytical methods is an integral part of the quality control system, being a critical process in the pharmaceutical industries to ensure the quality and safety of pharmaceutical products. In this work we present the validation of an analytical method for titration of Bisoprolol fumarate 2.5 mg coated tablet, using the high-performance liquid chromatography technique established in USP 2023. Among the statistical parameters used in the present validation are: Linearity; results are produced proportional to the concentration of the analyte, is demonstrated by a correlation coefficient of r= 0.999, (minimum permissible value = 0.997). Accuracy measures the closeness of the results achieved by this methodology and the true value. Using the student's test to demonstrate the accuracy of the analytical method, a texp (-0.097) was obtained, which is lower than the t of the tables (2.306); therefore, there is no significant difference between the average recovery and the added amount of analyte, that is to say the percentage recovery of the analyte is very close to 100%. The precision of the analytical method indicates the degree of agreement or dispersion of test results. The RSD values obtained (0.65% for repeatability and 0.93% for intermediate precision) demonstrate the precision of the analytical method (maximum allowable value, RSD = 2.0%). The method is specific, as the presence of degradation products of Bisoprolol fumarate was not detected when the active principle was subjected to different forced degradation procedures, therefore, the method is selective.
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Palabras clave
Validación, Precisión, Bisoprolol, Accuracy