RESUMO
A simple, rapid, cost effective and extractive UV spectrophotometric method was developed for the determination of Gemcitabine HCl (GMCT) in bulk drug and pharmaceutical formulation. It was based on UV spectrophotometric measurements in which the drug reacts with gold nanoparticles (AuNP) and changes the original colour of AuNP and forms a dark blue coloured solution which exhibits absorption maximum at 688nm. The apparent molar absorptivity and Sandell's sensitivity coefficient were found to be 3.95×10(-5)lmol(-1)cm(-1) and 0.060µgcm(-2) respectively. Beer's law was obeyed in the concentration range of 2.0-40µgml(-1). This method was tested and validated for various parameters according to ICH guidelines. The proposed method was successfully applied for the determination of GMCT in pharmaceutical formulation (parental formulation). The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation <2%). As it is simple, cheap and less time consuming, it can be suitably applied for the estimation of GMCT in dosage forms.
Assuntos
Antineoplásicos/análise , Técnicas de Química Analítica/métodos , Desoxicitidina/análogos & derivados , Ouro/química , Nanopartículas Metálicas/química , Nanotecnologia/métodos , Antineoplásicos/química , Desoxicitidina/análise , Desoxicitidina/química , Injeções , Luz , Limite de Detecção , Nanopartículas Metálicas/ultraestrutura , Tamanho da Partícula , Preparações Farmacêuticas , Reprodutibilidade dos Testes , Espalhamento de Radiação , Soluções , Espectrofotometria Ultravioleta , Espectroscopia de Infravermelho com Transformada de Fourier , GencitabinaRESUMO
A simple, rapid and sensitive method has been developed and validated for the determination of pramipexole in rat plasma by using gas chromatography mass spectrometry. The lower limit of quantification (LLOQ) is superior to the other reported LC-MS/MS methods. After being made alkaline with NaOH, plasma samples (0.1 mL) were subjected to liquid-liquid extraction using methyl-t-butyl ether. Analytes were determined using electron impact ionization in a single quadrupole mass spectrometer. GC/MS was performed in the selected ion monitoring mode using target ions at m/z 211, 212 and 152 for pramipexole and m/z 194 and 165 for caffeine as internal standard. A linear calibration curve was plotted over the range of 20-1000 pg/mL for pramipexole (r(2) > 0.996). The LLOQ was 20.0 pg/mL, respectively, which offered high sensitivity and selectivity enough for bioanalytical investigation. Inter- and intraday precisions ranged from 0.3 to 8.8% and from 0.9 to 11.33%, respectively. The recovery of pramipexole from plasma ranged from 82.4 ± 7.1 to 87.8 ± 5.7%. The method fulfills all standards required for bioanalytical methods and can be successfully applied to a pharmacokinetic study of pramipexole in rats.
