Validación de un método analítico por cromatografía líquida de alta resolución (HPLC) para la cuantificación de Dextrometorfano bromhidrato 7,5 mg en pastilla dura para chupar
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Date
2021
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Universidad Nacional de Trujillo
Abstract
El presente trabajo tiene como objetivo desarrollar y validar un método analítico para el producto Dextrometorfano bromhidrato 7,5 mg en pastilla dura para chupar elaborado en un laboratorio farmacéutico nacional mediante cromatografía de alta resolución en fase inversa RP-HPLC con detector DAD. Se logró la separación e identificación en 7 minutos de corrida, utilizando una columna Purospher START RP-18encaped (5 um) a temperatura de 25 °C con una fase móvil compuesta por Acetonitrilo grado HPLC, Metanol grado HPLC y Buffer pH 2,5 en proporción de 24:5:71, respectivamente. El volumen de inyección utilizada fue de 23 μL y una velocidad de flujo de 2,2 mL/min, el analito se detectó a una longitud de onda de 220 nm. Las muestras de producto fueron llevadas a condiciones extremas de estrés acido, alcalino, térmico, oxidativo y luz en los cuales se encontraron 5 productos de degradación. Los datos resultantes dieron conformidad de la linealidad de la metodología analítica dando un coeficiente de determinación (R2) de 0,9998 que cumple con lo establecido (>0.998) lo cual estadísticamente nos indica que existe proporcionalidad, así como la aptitud del sistema (RSD% 0,1054) con un RSD <2% y la precisión del método fue evaluado para demostrar su repetitividad resultando un RSD% de 0,2773 que es menor al criterio de evaluación (RSD%<2). El corroboró que el método es exacto mediante el estadístico t-Student (p<0,005, n-1 grados de libertad) para los porcentajes de recuperación teniendo un texp (1,079) menor al t tabla (2,306). Además, se estableció que el método tenía suficiente precisión intermedia, ya que se logró una separación similar con el mismo instrumento con diferentes operadores y diferentes días. Se logró validar con éxito el método para el análisis de Dextrometorfano bromhidrato 7,5 mg en pastilla dura para chupar. Además de cumplir con todos los parámetros de validación descritos en la USP
ABSTRACT The objective of this work is to develop and validate an analytical method for the product Dextromethorphan hydrobromide 7.5 mg hard lozenge prepared in a national pharmaceutical laboratory by means of high resolution reverse phase chromatography RP-HPLC with DAD detector. The separation and identification were achieved in 7 minutes of running, using a Purospher START RP-18encaped column (5 um) at a temperature of 25 ° C with a mobile phase composed of Acetonitrile grade HPLC, Methanol grade HPLC and Buffer pH 2.5 in ratio of 24: 5: 71, respectively. The injection volume used was 23 μL and a flow rate of 2.2 mL / min, the analyte was detected at a wavelength of 220 nm. The product samples were taken to extreme conditions of acid, alkaline, thermal, oxidative and light stress in which there were 5 degradation products. The resulting data gave conformity to the linearity of the analytical methodology, giving a coefficient of determination (R2) of 0.9998 that complies with the established (> 0.998) which statistically indicates that there is existence, as well as the proportional aptitude of the system (RSD % 0.1054) with an RSD <2% and the precision of the method was evaluated to demonstrate its repeatability, resulting in an RSD% of 0.2773 which is less than the evaluation criterion (RSD% <2). He confirmed that the method is accurate using the t-Student statistic (p <0.005, n-1 degrees of freedom) for the recovery percentages, having a texp (1.079) lower than the t table (2.306). Furthermore, it was established that the method had sufficient intermediate precision, since a similar separation was achieved with the same instrument with different operators and different days. The validated method was successfully used for the analysis of the pharmaceutical preparation in hard candy against cough, showing recovery and pressure. The method for the analysis of Dextromethorphan hydrobromide 7.5 mg in hard lozenge was successfully validated. In addition to complying with all the validation parameters described in the USP
ABSTRACT The objective of this work is to develop and validate an analytical method for the product Dextromethorphan hydrobromide 7.5 mg hard lozenge prepared in a national pharmaceutical laboratory by means of high resolution reverse phase chromatography RP-HPLC with DAD detector. The separation and identification were achieved in 7 minutes of running, using a Purospher START RP-18encaped column (5 um) at a temperature of 25 ° C with a mobile phase composed of Acetonitrile grade HPLC, Methanol grade HPLC and Buffer pH 2.5 in ratio of 24: 5: 71, respectively. The injection volume used was 23 μL and a flow rate of 2.2 mL / min, the analyte was detected at a wavelength of 220 nm. The product samples were taken to extreme conditions of acid, alkaline, thermal, oxidative and light stress in which there were 5 degradation products. The resulting data gave conformity to the linearity of the analytical methodology, giving a coefficient of determination (R2) of 0.9998 that complies with the established (> 0.998) which statistically indicates that there is existence, as well as the proportional aptitude of the system (RSD % 0.1054) with an RSD <2% and the precision of the method was evaluated to demonstrate its repeatability, resulting in an RSD% of 0.2773 which is less than the evaluation criterion (RSD% <2). He confirmed that the method is accurate using the t-Student statistic (p <0.005, n-1 degrees of freedom) for the recovery percentages, having a texp (1.079) lower than the t table (2.306). Furthermore, it was established that the method had sufficient intermediate precision, since a similar separation was achieved with the same instrument with different operators and different days. The validated method was successfully used for the analysis of the pharmaceutical preparation in hard candy against cough, showing recovery and pressure. The method for the analysis of Dextromethorphan hydrobromide 7.5 mg in hard lozenge was successfully validated. In addition to complying with all the validation parameters described in the USP
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Keywords
HPLC, validación, Dextrometorfano bromhidrato, detector DAD