A simple, rapid, economical and reliable high performance liquid chromatographic method has been developed and successfully applied in simultaneous determination of ethinyl estradiol and drospirenone in coated tablets. The HPLC method was performed on a LiChroCART ® 100RP column (125x4 mm i.d., 5 µm) with acetonitrile:water 50:50 (v/v) as mobile phase, pumped at a flow rate of 1.0 mL.min -1 . The fluorescence detection for ethinyl estradiol was made at λ ex = 280 nm and λ em = 310 nm and a UV detection for drospirenone was made at 200 nm. The elution time for ethinyl estradiol and drospirenone were 4.0 and 5.7 min, respectively. The method was validated in accordance to USP 34 guidelines. The proposed HPLC method presented advantages over reported methods and is suitable for quality control assays of ethinyl estradiol and drospirenone in coated tablets. Um método simples, rápido, econômico e confiável foi desenvolvido empregando a cromatografia líquida de alta eficiência para a determinação simultânea de etinilestradiol e drospirenona em comprimidos revestidos. O método foi realizado utilizando coluna LiChroCART ® 100RP (125 x 4 mm d.i., 5 µm), a fase móvel constituída de acetonitrila:água, 50:50 (v/v) com vazão de 1,0 mL.min -1 . A detecção foi realizada empregando fluorescência em λ ex = 280 nm e λ em = 310 nm para o etinilestradiol e na região de UV em 200 nm para a drospirenona. O etinilestradiol e a drospirenona tiveram tempo de retenção de 4,0 e 5,7 min, respectivamente. O método foi validado de acordo com as diretrizes da USP 34. O método proposto apresentou vantagens sobre os relatados na literatura e pode ser considerado adequado para o controle de qualidade do etinilestradiol e da drospirenona em comprimidos revestidos. Unitermos:Comprimidos revestidos/análise quantitativa. Cromatografia líquida de alta eficiência/ análise quantitativa. Etinilestradiol/determinação quantitativa. Drospirenona/determinação quantitativa. Detecção por fluorescência. Detecção no UV.
In this work, were performed qualitative and quantitative identitication econazole nitrate (raw material); thermal characterization of econazole nitra excipients and formulation (cream). There also were developed and validated spec and selective analytical methodology for quanlilative determination of econazole nitra in creams. The thermal characterization of drug product excipients was performed usi lhe Thermogravimetry (TG). For the thermal characterization of econazole nitrate dr and their formulation were used the Thermogravimetry, Derivative Thermogravime (TG/DTG) and Differential Scanning Calorimetry (DSC). From cream formulation we identified and quantitied two kinds of water which have differenl inleraclions wilh l matrix. As regards lo developing of specitic melhodology was used lhe capillary zo eleclrophoresis (CZE). The melhod was linear, wilh a correlalion coefficienl of 0.9995 lhe concenlration range of 80 to 120 J..Ig mL-i of econazole nilrate, precision calculat as relative slandard deviation (RSD) was less lhan 2%, accuracy calculaled percentage of recovery for commercial sample was of 100 ± 2.5%, delection a quantitation limits were 1.853 J..Ig mL-1 and 5.617 J..Ig mL-i , respectively. The CZE meth showed to be robust. For developing of selective methodology were used h performance liquid chromatography (HPLC) wilh gradienl elution, and mice electrokinelic chromatography (MEKC) melhods. Econazole nilrale, related impurities the drug (4-Chlorobenzyl alcohol, alpha-2 ,4-dichlorophenyl-1 H-imidazole-1-ethan and preservatives (melhylparaben, propylparaben) presenl in lhe drug product we separated. The HPLC method was linear for ali analytes, lhe correlalion coefficie were higher than 0.99. The precision for nitrate econazol in terms of RSD was less th 2%, lhe percentage of recovery for commercial sample of econazole nitrate was 100 2%, the method is robust and could be applied for the quantitation of the five substanc cited above. With the MEKC method developed the tive substances were separated less time comparated with HPLC method.
orientação, pelo apoio, pela confiança e pelo incentivo em nosso trabalho. Aos professores Maria Inês Rocha Miritello Santoro, María Segunda Aurora Prado e Jorge Luis Seferin Martins, pelo apoio e incentivo no dia a dia no laboratório. À Profa. Marina Franco Maggi Tavares, pelas sugestões, pelo incentivo e pela disposição brindada no decorrer deste trabalho. Aos professores Jivaldo do Rosário Matos e Lucildes Pita Mercuri, pelo incentivo, pelo apoio e pela amizade. Ao Prof. Anil Kumar Singh pelas sugestões no decorrer deste trabalho. Aos colegas de Laboratório, Pedro, Alessandra, Viviane, Cinthia, Claudia e Hellen, pelo companheirismo e pelo apoio. Aos meus colegas da Apsen Farmacêutica, pelo apoio e pela amizade no decorrer deste trabalho. A minha colega Patricia Lika Yamaguchi pelo apoio brindado. À funcionaria do laboratório, Iria, pela colaboração e pela amizade. Aos funcionários David, Elizabete Paiva, Elaine Ychico e em especial ao Jorge pela colaboração e pela amizade. À funcionaria Leila Aparecida Bonadio, da Biblioteca do Conjunto das Químicas, pela revisão das referências utilizadas nesta pesquisa. À FAPESP, pelo apoio financeiro concedido. A todos que, de alguma forma, colaboraram para a realização deste trabalho. Muito Obrigado. Palavras chaves: Método indicador de estabilidade, cromatografia líquida de alta eficiência, eletroforese capilar, degradação forçada, produtos de degradação.
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