RESUMO
A robust colourimetric flow injection analysis (FIA) procedure is described for the determination of busulphan in dissolution samples of a 2 mg tablet formulation. The sample solution is injected directly into a reagent stream containing 4-(4-nitrobenzyl)pyridine/potassium hydrogen phthalate. An on-line heating stage allows the formation of a coloured pyrridinium salt species, which following stabilisation is detected spectrophotometrically at 570 nm. The method has been fully validated and is linear over the concentration range 0.004-0.024 mg of busulphan ml(-1). The method can also been applied to uniformity of content and bulk assay testing.
Assuntos
Bussulfano/análise , Colorimetria , Estudos de Avaliação como Assunto , Análise de Injeção de Fluxo/métodos , Piridinas/química , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Espectrofotometria , ComprimidosRESUMO
A flow injection analysis (FIA) procedure is described for the determination of pentavalent antimony (Sb5+) in the drug, sodium stibogluconate, in a parenteral pharmaceutical formulation. The sample solution is injected directly into a carrier stream of iodide ion which is then mixed with an acid stream in situ. Sb5+ is determined by the redox reaction with acidified iodide to liberate iodine, which is monitored spectrophotometrically at 350 nm. The closed conditions prevent interference from atmospheric oxygen and the rapid reaction time assists in minimizing interference from side reactions. The use of tartaric acid as a solvent for sample and standard solutions ensures obedience of Beer's law over the Sb5+ concentration range 0.01-0.2% (w/v). The method is specific for the higher oxidation state in an ionic mixture of Sb5+ and Sb3+, and has been fully validated for use in a pharmaceutical preparation. Assuming absence of matrix interference it is applicable to Sb5+ from other sources and should be applicable to other reducible ionic species.
