Development and validation of a method for the determination of valproic acid in pharmaceutical formulations by high performance liquid chromatography with diode array detection (HPLC-DAD)

• Autor(a) principal: Souza, Paulo Ricardo de Souza e
• Data de Publicação: 2013
• Outros Autores: Carvalho, Juliana Machado de, Albert, André Luis Mazzei, Moreira, Josino Costa, Leandro, Katia Christina
• Tipo de documento: Artigo
• Idioma: eng
• Título da fonte: Vigilância Sanitária em Debate
• Texto Completo: https://visaemdebate.incqs.fiocruz.br/index.php/visaemdebate/article/view/16
• topic: cromatografia líquida de alta eficiência acoplada com detector de conjunto de fotodiodos; ácido valpróico; validação; high performance liquid chromatography; HPLC-DAD; valproic acid; validation

Valproic acid (VA) is used as an anticonvulsant and is used in the treatment of bipolar disorder and depression. The official analytical method for this drug in the compendia is gas chromatography, which is unavailable in many quality control laboratories. Here, we report a validated alternative method using high performance liquid chromatography with diode array detection (HPLC-DAD). The optimized parameters and conditions were as follows: C18 column (5 µm; 250 x 4 mm d.i.); flow 1.0 mL.min-1; wavelength: 210 nm; mobile phase: 55% acetonitrile (ACN) in water containing 0.05% v/v trifluoroacetic acid (TFA) (v/v). The analytical parameters that were validated included the selectivity and matrix effects, linearity, repeatability and intermediate, precision, accuracy, recovery and robustness. This method identifies VA unambiguously. In validation, the following results were obtained: good linearity in concentrations between 0.7 and 1.3 mg.mL-1 (r2 = 0.9998), relative standard deviations (RSDs) of 0.68% for repeatability and 1.23% for intermediate precision, a recovery of 99.42 to 101.55% (RSD 0.14 to 0.74%) and an accuracy of 100.68% (RSD = 0.79%). This method is robust to small variations in procedure.