RESUMO
Guanylhydrazones are molecules with great pharmacological potential in various therapeutic areas, including antitumoral activity. Factorial design is an excellent tool in the optimization of a chromatographic method, because it is possible quickly change factors such as temperature, mobile phase composition, mobile phase pH, column length, among others to establish the optimal conditions of analysis. The aim of the present work was to develop and validate a HPLC and UHPLC methods for the simultaneous determination of guanylhydrazones with anticancer activity employing experimental design. Precise, exact, linear and robust HPLC and UHPLC methods were developed and validated for the simultaneous quantification of the guanylhydrazones LQM10, LQM14, and LQM17. The UHPLC method was more economic, with a four times less solvent consumption, and 20 times less injection volume, what allowed better column performance. Comparing the empirical approach employed in the HPLC method development to the DoE approach employed in the UHPLC method development, we can conclude that the factorial design made the method development faster, more practical and rational. This resulted in methods that can be employed in the analysis, evaluation and quality control of these new synthetic guanylhydrazones.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Hidrazonas/análise , Hidrazonas/química , Limite de Detecção , Peso MolecularRESUMO
This paper describes the development and validation of a HPLC-UV method (210 nm) for the simultaneous quantitation of artemether and lumefantrine in fixed dose combination tablets. The method showed to be linear (r(2)>0.99), precise (R.S.D.<2.0%), accurate (recovery of 101.07% for artemether and 101.58% for lumefantrine), specific and robust. Four batches of artemether-lumefantrine tablets were assayed by the validated method. The artemether contents in the tablets varied from 98.61% to 103.35%, while lumefantrine contents were 97.92-100.48%.
