RESUMO
Three process-related impurities were observed in routine monitoring of the samples by HPLC. These impurities were identified by LC-MS. One of the impurities, Imp-3 [rizatriptan-2,5-dimer] was reported in literature. Other two impurities were isolated by preparative HPLC and characterized by NMR, Mass and IR. Pure impurities obtained by isolation were co-injected with Rizatriptan benzoate sample to confirm the retention times in HPLC. Structure elucidation of these impurities by spectral data has been discussed in detail. These impurities were identified as 4-(5-((1H-1,2,4-triazol-1-yl)methyl)-3-(2-(dimethylamino)ethyl)-1H-indol-1-yl)-4-(5-((1H-1,2,4-triazol-1-yl)methyl)-3-(2-(dimethylamino)ethyl)-1H-indol-2-yl)-N,N-dimethylbutan-1-amine [rizatriptan-1,2-dimer] and [4,4-bis-(5-((1H-1,2,4-triazol-1-yl)methyl)-3-(2-(dimethylamino)-ethyl)-1H-indol-2-yl)-N,N-dimethylbutan-1-amine [rizatriptan-2,2-dimer].
Assuntos
Contaminação de Medicamentos , Agonistas do Receptor de Serotonina/química , Triazóis/química , Triptaminas/química , Cromatografia Líquida de Alta Pressão/métodos , Espectroscopia de Ressonância Magnética/métodos , Espectrometria de Massas/métodos , Estrutura Molecular , Reprodutibilidade dos Testes , Agonistas do Receptor de Serotonina/análise , Agonistas do Receptor de Serotonina/normas , Espectrofotometria Infravermelho/métodos , Triazóis/análise , Triazóis/normas , Triptaminas/análise , Triptaminas/normasRESUMO
Impurity profiling of dicloxacillin sodium bulk drug and pharmaceutical dosage forms subjected to stability studies is evaluated. Of many impurities detected in HPLC analysis, three were not reported in the literature. The impurities have been identified by LC-MS; isolated by preparative HPLC; and characterised by NMR, Mass spectroscopy and IR. Pure impurities obtained by isolation were co-injected with dicloxacillin sodium sample to confirm the retention times in HPLC. Structure elucidation of these degradation products by spectral data has been discussed in detail.