RESUMO
An isocratic chiral HPLC method was developed for the separation of tolterodine tartarate enantiomers. The mobile phase consists of n-hexane and isopropyl alcohol in the ratio of 980:20 (v/v) with 1 ml diethylamine and 0.6 ml trifluoroacetic acid. Chiralcel OD-H (250 mm x 4.6mm) column was used at constant room temperature. Flow rate was kept at 0.5 ml/min. This method is capable of detecting the S-isomer up to 0.1 microg/ml. The method was validated in terms of linearity, precision, limit of detection (LOD) and limit of quantification (LOQ).
Assuntos
Compostos Benzidrílicos/química , Cresóis/química , Fenilpropanolamina/química , Cromatografia Líquida de Alta Pressão , Estrutura Molecular , Reprodutibilidade dos Testes , Estereoisomerismo , Tartarato de TolterodinaRESUMO
During the impurity profile of Celecoxib, four polar impurities (impurity I, II, III and IV) and one non-polar impurity (impurity V) with respect to Celecoxib were detected by HPLC. LC-MS has been employed in this impurity profile study. The three polar impurities (I, II and III) were found to be process related while impurities (IV and V) turned out to be isomers. The impurities III, IV and V were isolated with the help of preparative HPLC. The structure of impurities III, IV (ortho-isomer) and V (regio-isomer) were confirmed as [5-(4-methylphenyl)-3-trifluoromethyl-1H-pyrazole], 4-[5-(2'-methyl phenyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl] benzenesulfonamide, and 4-[4-(4'-methylphenyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl]-benzenesulfonamide, respectively. The structures of impurities I, II, III and IV were confirmed by synthesis and structural characterization using spectral data. However, the impurity V was not synthesized.
Assuntos
Inibidores de Ciclo-Oxigenase/síntese química , Inibidores de Ciclo-Oxigenase/isolamento & purificação , Contaminação de Medicamentos , Isoenzimas/antagonistas & inibidores , Pirazóis/síntese química , Pirazóis/isolamento & purificação , Sulfonamidas/síntese química , Sulfonamidas/isolamento & purificação , Celecoxib , Cromatografia Líquida de Alta Pressão/métodos , Ciclo-Oxigenase 2 , Inibidores de Ciclo-Oxigenase 2 , Espectrometria de Massas/métodos , Prostaglandina-Endoperóxido SintasesRESUMO
In the synthesis of Moxifloxacin four prominent impurities were detected in HPLC analysis. These impurities were detected in gradient HPLC method. They were isolated from enriched mother liquors and were characterized as 1-cyclopropyl-6-fluoro-1,4-dihydro-8-methoxy-7-[(S,S)-N-methyl-2,8-diazabicyclo (4,3,0) non-8yl]-4-oxo-3-quinoline carboxylic acid (Impurity-1), methyl-1-cyclopropyl-6-fluoro-1,4-dihydro-8-methoxy-7-[(S,S)-2,8-diazabicyclo(4,3,0)non-8-yl]-4-oxo-3-quinoline carboxylate (impurity-2), and 1-cyclopropyl-6-fluoro-1,4 dihydro-8-hydroxy-7-[(S,S)-2,8-diazobicyclo(4,3,0)non-8-yl]-4-oxo-3-quinoline carboxylicacid (impurity-3), 1-cyclopropyl-6,7-difluoro-8-hydroxy-4-oxo-1,4 dihydro-3-quinoline carboxylicacid (impurity-4) by means of 1H, 13C NMR, DEPT, IR and mass spectral data. Structural elucidation by spectral data was discussed.
Assuntos
Compostos Aza/análise , Compostos Aza/química , Contaminação de Medicamentos , Quinolinas/análise , Quinolinas/química , Cromatografia Líquida de Alta Pressão , Fluoroquinolonas , Espectroscopia de Ressonância Magnética , Espectrometria de Massas/métodos , Estrutura Molecular , Moxifloxacina , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
Three unknown impurities in loratadine bulk drug at levels below 0.1% (ranging from 0.05 to 0.1%) were detected by a simple isocratic reversed-phase high performance liquid chromatography (HPLC). These impurities were isolated from mother liquor sample of loratadine using reversed-phase preparative HPLC. Based on the spectral data (IR, NMR and MS) the structures of these impurities were characterized as 11-(N-carboethoxy-4-piperidylidene)-6,11-dihydro-5H-benzo(5,6) cyclopenta(1,2-b)-pyridine (I), 8-bromo-11-(N-carboethoxy-4-piperidylidene)-6,11-dihydro-5H-benzo(5,6) cyclopenta (1,2-b)-pyridine (II) and 8-chloro-11-(N-carboethoxy-4-piperidylidene)-5H-benzo(5,6) cyclopenta (1,2-b)-pyridine (III). The synthesis of these impurities was discussed.
Assuntos
Antagonistas não Sedativos dos Receptores H1 da Histamina/química , Loratadina/química , Cromatografia Líquida de Alta Pressão , Contaminação de Medicamentos , Antagonistas não Sedativos dos Receptores H1 da Histamina/análise , Loratadina/análise , Espectroscopia de Ressonância Magnética , Espectrometria de Massas , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
In the impurity profile of mosapride a polar impurity (0.1%) was detected in HPLC with respect to mosapride. Based on the mass spectral data obtained by LC-MS/MS analysis this impurity structure was characterised as 4-amino-5-chloro-2-ethoxy-N-[[(4-benzyl)-2-morphinyl] methyl] benzamide. It is interesting to note that this impurity is potent analogue of mosapride, which will have much higher gastroprokinetic activity than metoclopramide. This impurity was synthesised from an unambiguous route and confirmed the structure by collecting various spectral data and the formation is discussed. To our knowledge this compound was not reported as process impurity elsewhere.
