Validación de un método de muestreo y análisis para la cuantificación del haloperidol en residuos de limpieza de los equipos de producción de la industria farmacéutica

Abstract

A sampling and analysis procedure of haloperidol cleaning residue that remain on surface of the manufacturing equipment was developed and validated. These procedure will be use in cleaning validation equipment for to ensure that haloperidol content is in pre-determined acceptable level. A linear, accurate and precise analytical method by HPLC was employed to quantify in the interval
of 3 to 11 ppm. The detection and quantitation limits values were 1.25 and 2.5 ppm, respectively. Sampling and analysis procedure was specific for the analyte in presence of possible interferences like excipients, recovery solvent and swap material. The excipients and active ingredient were treated in the most drastic cleaning conditions. After treatment it was obtained that placebo no interfere in
haloperidol determination. Also it was determined, that there is not degradation of active ingredient during treatment realized, so there are not interferences due to degradation products. An accuracy and repeatability assay for the whole procedure was carried out. In this assay for five analyzed concentrations a total mean and a total variation coefficient of recoveries of 85.11 and 3.32 %, respectively were obtained. The lost analyte during complete procedure was approximately of 15 % but as this bias is constant in the range of analyzed concentrations, the result can be corrected without problems.