Development and validation of analytical methodology for quantifying sodium and calcium in lithium carbonate using the ICP OES technique with automated sampling

Abstract

The validation process of analytical methodologies in research laboratories is essential for obtaining approval from ANVISA (Brazilian Health Regulatory Agency) and, consequently, for the registration and commercialization of drugs, whether they are reference or generic. This involves conducting specific tests on Active Pharmaceutical Ingredients (APIs), which must meet the specifications in pharmacopoeias and/or recognized compendia or, if necessary, validated methods that have been performed and proven to be efficient. In this context, the work aims to validate an analytical methodology for quantifying Calcium and Sodium in the raw material Lithium Carbonate, using the ICP-OES technique with the evaluation of various parameters, including selectivity, linearity, limit of quantification, precision (repeatability and intermediate), accuracy, working range, and robustness. The goal is to ensure that the method meets the requirements of current legislation. To perform the analyses, the samples were prepared by dissolving them in a 5 mol L-1 hydrochloric acid solution. The results demonstrated that the analytical method is capable of identifying and quantifying the analytes of interest without spectral interferences, maintaining a direct relationship between concentration and analytical response, and exhibiting precision and accuracy under the specified experimental conditions.