Acceso usuarios
Kelly Johana Rojas, Natalia Afanasjeva
Introducción. En la industria farmacéutica la cuantificación de trazas de principios activos de los medicamentos es crucial para validar los procesos de limpieza post-fabricación, debido al riesgo de contaminación cruzada cuando se ejecuta un proceso de limpieza inadecuado. Objetivo. Validar una metodología analítica en condiciones del clima tropical para cuantificar trazas de medicamento antiinflamatorio no esteroideo (AINES) o Meloxicam en equipos de fabricación utilizando cromatografía líquida de alta eficiencia (HPLC). Metodología. Se empleó una columna Zorbax Eclipse XDB-C18 (4.6 x 150 mm, 5 µm, Agilent) a 30°C ± 2°C, donde la fase móvil consistió en un 90% de un buffer fosfato de amonio monobásico (pH=7.0) con 2-propanol y metanol, y un 10% de metanol, a un flujo de 1,0 mL/min, la detección se realizó a 360 nm, con un volumen de inyección de 10 µL, y como diluente se usó la misma fase móvil.
Introduction. In the pharmaceutical industry, the quantification of trace amounts of active ingredients in drugs is essential to validate post-manufacturing cleaning processes, given the risk of cross-contamination resulting from inadequate cleaning process. Objective. To validate an analytical methodology in tropical climate conditions to quantify traces of the non-steroidal anti-inflammatory drug (NSAID) or Meloxicam in manufacturing equipment using high performance liquid chromatography (HPLC). Methodology. The analysis was carried out on Zorbax Eclipse XDB-C18 column (4.6 x 150 mm, 5 µm, Agilent) at 30°C ± 2°C. The mobile phase consisted of 90% monobasic ammonium phosphate buffer (pH 7.0) with 2-propanol and methanol, and 10% methanol, at a flow rate of 1.0 mL/min. Detection was performed at 360 nm, with an injection volume of 10 µL, and the same mobile phase was used as diluent. Results. The method showed excellent linearity, with a statistical correlation coefficient R ≥ 0.999. The coefficient of variation did not exceed the RSD limit of 13% in the repeatability of the system in all the surfaces evaluated and in intermediate precision the criterion of RSD < 20.0% was fulfilled. Accuracy test yielded a recovery percentage above the acceptance criterion of 50%. There were no interferences in the specificity. Conclusions. The studies performed validate the proposed HPLC methodology for the quantification of Meloxicam traces by HPLC, showing that is precise, accurate, selective, efficient, robust and suitable to carry out in pharmaceutical analysis laboratories. Moreover, the optimization of critical parameters un tropical climate conditions, such as filter type, time and nature of the extraction solvent, as well as the stability of the method, also provided a solid basis for its implementation in the quality control area.
