RESUMO
A stability indicating UPLC method was developed and validated for the simultaneous determination of atorvastatin, fenofibrate and their impurities in tablets. The chromatographic separation was performed on acquity UPLC BEH C18 column (1.7 microm, 2.1 mmx100 mm) using gradient elution of acetonitrile and ammonium acetate buffer (pH 4.7; 0.01 M) at flow rate of 0.5 ml/min. UV detection was performed at 247 nm. Total run time was 3 min within which main compounds and six other known and major unknown impurities were separated. Stability indicating capability was established by forced degradation experiments and separation of known degradation products. The method was validated for accuracy, repeatability, reproducibility and robustness. Linearity, LOD and LOQ was established for atorvastatin, fenofibrate and their known impurities.
Assuntos
Anticolesterolemiantes/análise , Cromatografia Líquida de Alta Pressão/métodos , Contaminação de Medicamentos/prevenção & controle , Fenofibrato/análise , Ácidos Heptanoicos/análise , Pirróis/análise , Anticolesterolemiantes/química , Anticolesterolemiantes/metabolismo , Atorvastatina , Soluções Tampão , Estabilidade de Medicamentos , Fenofibrato/química , Fenofibrato/metabolismo , Ácidos Heptanoicos/química , Ácidos Heptanoicos/metabolismo , Concentração de Íons de Hidrogênio , Estrutura Molecular , Pirróis/química , Pirróis/metabolismo , Padrões de Referência , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Comprimidos , Fatores de TempoRESUMO
A fast, robust and stability indicating RP-HPLC method was developed for simultaneous determination of bisoprolol fumarate and amlodipine besylate in tablets. The mobile phase was mixture of 25 mM ammonium acetate adjusted to pH 5.0 and methanol (65: 35) at 0.8 ml/min. The stationary phase was Luna C18-2 column (3 mu, 50x4.6 mm ID). UV detection was performed at 230 nm. Retention time was 1.45 min and 3.91 min for bisoprolol and amlodipine, respectively. Linearity was established in the range of 8-33 mug/ml. Mean recovery was 99.1% and 98.6% for bisoprolol fumarate and amlodipine besylate, respectively.
