Validação de método analítico para impurezas elementares para o comprimido revestido de riluzol 50 mg

Abstract

For several years the control of elemental impurities recommended in the pharmacopoeia was the colorimetric method of heavy metals. Due to the lack of selectivity, low and varied recovery, among others problems, it was necessary to use more robust and sensitive techniques, capable of quantifying each impurity individually. Thus, since January 2018, the pharmacopoeias have replaced the colorimetric technique with the instrumental techniques of Inductively Coupled Plasma Optical Emission Spectrometry and Inductively Coupled Plasma Mass Spectrometry (ICP-OES and ICP-MS). Non-compendial analytical methods require analytical validation as required by RDC nº 166/2017. Therefore, the objective of this work is to validate an analytical methodology for the quantification of cadmium, lead, arsenic, mercury, cobalt, vanadium and nickel in coated tablets of riluzole 50 mg using the ICP-OES technique. The samples were prepared using microwave-assisted decomposition technique. The analytical method was able to identify and quantify the analytes of interest without spectral interferences, diluents and matrix components, presented analytical responses directly proportional to the concentration and proved to be accurate and accurate under the established experimental conditions.