RESUMO
To develop a sensitive and specific high performance liquid chromatography-tandem mass spectrometric (HPLC-MS/MS) method for the determination of mosapride in human plasma, mosapride and internal standard tamsulosin were extracted from plasma with liquid-liquid extraction, then separated on a Waters ACQUITY UPLC BEH C18 column (50 mm x 2.1 mm, 1.7 microm ID) with gradient elution at flow-rate of 0.25 mL x min(-1). The mobile phase was water (containing 0.3% formic acid) and acetonitrile under gradient conditions. Electrospray ionization (ESI) source was applied and operated in the positive ion mode. Multiple reaction monitoring (MRM) mode with the transitions of m/z 422 --> m/z 198 and m/z 409 --> m/z 228 were used to quantify mosapride and the internal standard, respectively. The linear calibration curve was obtained in the concentration range of 0.17 - 68.00 ng x mL(-1). The lower limit of quantification was 0.17 ng x mL(-1). The inter- and intra-day precision (RSD) was less than 13%, and the accuracy (RE) was within +/- 6.3% calculated from QC samples. The method was used to determine the concentration of mosapride in plasma after a single oral dose of 5 mg mosapride citrate to 20 healthy male Chinese volunteers. The method has been proved to be selective, sensitive, rapid and suitable for pharmacokinetic study of mosapride.
Assuntos
Humanos , Masculino , Administração Oral , Área Sob a Curva , Benzamidas , Sangue , Farmacocinética , Cromatografia Líquida de Alta Pressão , Métodos , Fármacos Gastrointestinais , Sangue , Farmacocinética , Morfolinas , Sangue , Farmacocinética , Sensibilidade e Especificidade , Agonistas do Receptor de Serotonina , Sangue , Farmacocinética , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas em Tandem , MétodosRESUMO
<p><b>OBJECTIVE</b>To investigate the chemical constituents of Epimedium brevicornum.</p><p><b>METHOD</b>The chemical constituents were isolated by using silica gel column chromatography and preparative TLC. The structures were identified on the basis of physical-chemical constants and spectral data.</p><p><b>RESULT</b>Five compounds were isolated and identified as hyperoside, icariin, epimedin B, epimedin C, inositol.</p><p><b>CONCLUSION</b>Compound I and III - V were isolated from the plant for the first time.</p>