RESUMO
A capillary electrophoresis method was developed to determine the impurity of etodolac enantiomers. (2-Hydroxypropyl)-beta-cyclodextrin (HP-beta-CD) was used as a chiral selector and ketoprofen as an internal standard to improve the peak area precision. The seperation of the etodolac enantiomers was achived within 35 min at 15 degrees C and its highest resolution was about 4.0 using phosphate buffer (0.1 M, pH 6.0) with 15 mM HP-beta-CD and UV detection at 225 nm with a reference wavelength at 360 nm. This method allowed determination of 0.2% of (R)-(-)-etodolac in (S)-(+)-etodolac and method validation showed adequate linearity over the required range.
Assuntos
Anti-Inflamatórios não Esteroides/química , Etodolac/química , beta-Ciclodextrinas/química , 2-Hidroxipropil-beta-Ciclodextrina , Soluções Tampão , Eletroquímica , Eletroforese Capilar , Excipientes , Concentração de Íons de Hidrogênio , Padrões de Referência , Reprodutibilidade dos Testes , Estereoisomerismo , TemperaturaRESUMO
A new chiral derivatization agent with sugar moiety, 2,3,4,6-tetra-O-acetyl-beta-D-galactopyranosyl isothiocyanate (GATC) was synthesized. Several beta-blockers were investigated for the possible separation of the enantiomers by reversed-phase HPLC after derivatization with this new chiral derivatization agent (GATC). GATC was reacted readily with beta-blockers at room temperature and the reaction mixture could directly be injected into the HPLC system. The corresponding diastereomers were well resolved on an ODS column with acetonitrile-ammonium acetate buffer as a mobile phase and monitored at UV 254 nm. The optimization of the derivatization procedure (concentration of GATC, reaction temperature and time) and HPLC conditions (pH and ionic strength of mobile phase) were investigated and compared with GITC.
