RESUMO
A simple, rapid and reliable liquid chromatography coupled with quadrupole time of flight mass spectrometry (LC-Q-TOF-MS/MS) method was developed and validated for simultaneous determination of darunavir and its metabolites in rat serum and urine. The separation was accomplished on an Agilent RP-18 (250×4.6mm, 5µm) column using 20mM ammonium acetate and methanol (40:60, v/v) as a mobile phase at a flow rate of 1.0mL/min in an isocratic mode. The [M+H](+) ions of darunavir (m/z 548) and metabolites-I (m/z 392) were monitored in positive mode of ionization, while [M-H](-) ion of metabolite-II (m/z 172) in negative mode selectively. The matrix effects of rat serum and urine were found to be negligible and the recoveries were 87-93% for all the analytes. The short and long term stability of darunavir and its metabolites was within acceptable limits and the lower limits of quantification were in the range of 3.63-5.24ng/mL with a linear range of 5-5000ng/mL in rat serum as well as urine. The method exhibited good intra- and inter-day performance in terms of 2.54-8.92% precision and 0-5% accuracy. The method was successfully applied to a single-dose pharmacokinetic study of darunavir boosted with ritonavir in Wistar rats.
Assuntos
Sulfonamidas/sangue , Sulfonamidas/urina , Animais , Cromatografia Líquida/métodos , Darunavir , Estabilidade de Medicamentos , Ratos , Ratos Wistar , Sensibilidade e Especificidade , Sulfonamidas/farmacocinética , Espectrometria de Massas em Tandem/métodosRESUMO
A robust and sensitive solid-phase extraction followed by liquid chromatography-electrospray ionization mass spectrometric (LC-ESI-MS) method for determination of antibiotics viz., fluoroquinolones, sulfamethoxazole, trimethoprim and cephalosporines in surface waters was developed. The sample recoveries on Oasis HLB cartridges were found to be >80%. Identification was carried out by LC-ESI-MS/MS. The positive ion ESI mass spectra containing the peaks of quasimolecular ions [M+H](+) allowed the determination of molecular masses whereas the fragment ions obtained by MS/MS of [M+H](+) ions permitted the structural assignment. Quantification was carried out by selective ion monitoring (SIM) using the quasimolecular ions [M+H](+) of the parent compounds. The detection and quantification limits were found to be in the range of 0.6-8.1 and 2.0-24.0 microg/L. The surface waters of different lakes and tanks of Hyderabad, India were found to contain a few antibiotics.
Assuntos
Antibacterianos/análise , Cromatografia Líquida/métodos , Extração em Fase Sólida/métodos , Espectrometria de Massas por Ionização por Electrospray/métodos , Poluentes Químicos da Água/análise , Cefalosporinas/análise , Fluoroquinolonas/análise , Concentração de Íons de Hidrogênio , Combinação Trimetoprima e Sulfametoxazol/análiseRESUMO
A reversed-phase high performance liquid chromatographic (RP-HPLC) method for evaluation of purity of tamsulosin in bulk drugs and pharmaceuticals was developed. The separation was accomplished on an Inertsil C(18) column using 10 mM ammonium acetate: acetonitrile as a mobile phase in a gradient elution mode. A photodiode array detector set at 280 nm was used for detection. The impurities were identified by ESI-MS-MS. The detection limits were 0.06-0.11 microg/ml. The method was validated with respect to accuracy, precision, linearity, ruggedness and limits of detection and quantification. It finds application not only for monitoring the reactions during the process development but also on quality assurance of tamsulosin.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Espectrometria de Massas por Ionização por Electrospray/métodos , Sulfonamidas/análise , Espectrometria de Massas em Tandem/métodos , Soluções Tampão , Cromatografia Líquida de Alta Pressão/instrumentação , Contaminação de Medicamentos/prevenção & controle , Indústria Farmacêutica/instrumentação , Indústria Farmacêutica/métodos , Concentração de Íons de Hidrogênio , Estrutura Molecular , Preparações Farmacêuticas/análise , Preparações Farmacêuticas/química , Preparações Farmacêuticas/isolamento & purificação , Reprodutibilidade dos Testes , Espectrometria de Massas por Ionização por Electrospray/instrumentação , Sulfonamidas/química , Sulfonamidas/isolamento & purificação , Tansulosina , Espectrometria de Massas em Tandem/instrumentação , TemperaturaRESUMO
An extensive survey of the literature published in various analytical and pharmaceutical chemistry related journals has been conducted and the instrumental analytical methods which were developed and used for determination of COX-2 inhibitors in bulk drugs, formulations and biological fluids have been reviewed. This review covers the time period from 1995 to 2004 during which 138 analytical methods including all types of spectrophotometric and chromatographic techniques were reported. HPLC with UV detection was found to be the technique of choice for many workers and more than 100 methods were based on LC and UV. A critical analysis of the reported data has been carried out and the present state-of-art of the analytical techniques for determination of celecoxib, rofecoxib, etoricoxib, etodolac, nimesulide and meloxicam has been discussed.