Validation of a Method for Assay of Trifluoroacetates in the Pharmaceutical Substance Glatiramer Acetate by 19F NMR Spectroscopy

Abstract

A procedure for validation of an assay method for fluorine in residual trifluoroacetates in the pharmaceutical substance glatiramer acetate by ¹⁹F NMR spectroscopy is described. The method provides for assay of the content of trifluoroacetates without destruction of the substance under analysis. The validation process established the detection limit and assessed the linearity, accuracy, convergence, intralaboratory precision, and specificity of the method under validation. Measurement of “found:added” coefficients were used to calculate standard deviations, coefficients of variation, significance intervals, and systematic errors, using Fisher’s F test and Student’s t test to assess the assay results. The statistical characteristics were found to satisfy the criteria for acceptability of the validation parameters given in Russian and foreign normative documentation.