RESUMO
A high-performance liquid chromatographic (HPLC) method is described for the determination of ibuprofen in isolated erythrocytes and plasma. Before HPLC analysis ibuprofen was isolated by liquid-liquid extraction from these biological matrices; methylene chloride proved to be the best of the organic solvents tested. For the sample of erythrocytes it was necessary to carry out haemolysis prior to their extraction. HPLC was performed on a C-18 column with a mobile phase of methanol-water (220:100, v/v) acidified with perchloric acid to pH 3. Ultraviolet detection was at 222 nm. This method has been applied to the quantification of ibuprofen in rabbit erythrocytes and plasma for a pharmacokinetics study.
Assuntos
Anti-Inflamatórios não Esteroides/sangue , Eritrócitos/química , Ibuprofeno/sangue , Animais , Anti-Inflamatórios não Esteroides/farmacocinética , Cromatografia Líquida de Alta Pressão , Ibuprofeno/farmacocinética , Modelos Lineares , Coelhos , Sensibilidade e EspecificidadeRESUMO
A precise, accurate, reproducible one-step method for the high-performance chromatographic determination of ibuprofen in whole blood is described. Samples were, after haemolysis, prepared by solid-phase extraction. Analyses were performed using reversed-phase chromatography on a Separon SGX C18 column with a mobile phase of methanol-water (pH 3) and ultraviolet detection at 222 nm. The method was used for pharmacokinetic studies in rabbits.
Assuntos
Ibuprofeno/sangue , Animais , Cromatografia Líquida de Alta Pressão , Ibuprofeno/administração & dosagem , Ibuprofeno/farmacocinética , Indicadores e Reagentes , Indometacina/sangue , Injeções Intravenosas , Coelhos , Espectrofotometria UltravioletaRESUMO
A method using liquid-liquid extraction has been developed for the isolation of acetylsalicylic acid and its metabolites, salicylic, gentisic or possibly salicyluric acids, from whole blood, isolated erythrocytes and plasma. Methylene chloride proved to be the best of the organic solvents tested. For whole blood and isolated erythrocytes it was necessary to carry out haemolysis prior to their extraction. The high-performance liquid chromatographic conditions for the quantitation of acetylsalicylic acid and its metabolites from samples of whole blood, erythrocytes and whole plasma were optimized. Separation was performed using reversed-phase chromatography on Separon SGX C18 and ultraviolet detection at 236 nm. A mixture of methanol-water (80:100, v/v) was the mobile phase, acidified with perchloric acid to pH 2.5.
Assuntos
Eritrócitos/química , Gentisatos , Salicilatos/sangue , Animais , Aspirina/sangue , Células Cultivadas , Cromatografia Líquida de Alta Pressão , Hipuratos/sangue , Hidroxibenzoatos/sangue , Coelhos , Reprodutibilidade dos Testes , Ácido Salicílico , Espectrofotometria UltravioletaRESUMO
The stability of sulphamethoxydiazine (1) in HCl (1 mol/l) under elevated temperature was investigated. Isolated decomposition products further served as standards for the selection of HPLC conditions. Three types of stationary phases were tested: Pragosil 5, MicroPak CN-10, MicroPak CH-10. The selection of mobile phases was made in such a way as to be able to inject 1 hydrolysate in HCl (1 mol/l) directly or after simple dilution. Detection was performed with an UV detector at the wavelength of 226 nm. A column packed with MicroPak CN-10 was selected to investigate the process of 1 decomposition. The method made it possible to quantify 1 in the course of hydrolysis and to illustrate the process of decomposition. On the basis of continuous examination of the development of decomposition products during the stability study it was possible to consider the chemism of the decomposition reaction.
