6533b831fe1ef96bd1299929

RESEARCH PRODUCT

Chromatographic separation of chlorthalidone enantiomers using β-cyclodextrins as chiral additives

Rosa Herráez-hernándezPilar Campíns-falcó

subject

Beta-Cyclodextrinschemistry.chemical_compoundSpectrophotometrymedicineHumansDiureticsTriethylaminechemistry.chemical_classificationDetection limitCyclodextrinsChromatographyCyclodextrinmedicine.diagnostic_testbeta-CyclodextrinsChlorthalidoneStereoisomerismGeneral ChemistrySolutionschemistrySolventsIndicators and ReagentsSpectrophotometry UltravioletChlorthalidoneMethanolEnantiomermedicine.drug

description

Different beta-cyclodextrins have been tested as chiral additives in the mobile phase for the chromatographic analysis of chlorthalidone enantiomers in a C18 LiChrospher (125 x 4 mm I.D.) column. The effect on enantioresolution of different parameters was studied: composition of the mobile phase (percentage of organic solvent, type of buffer and pH), mobile phase flow-rate, and type and concentration of beta-cyclodextrin. A 25:75 mixture of methanol and 0.1 M phosphate buffer, pH 4, containing 2% triethylamine (v/v), and 12.5 mM beta-cyclodextrin, at a flow-rate of 0.8 ml/min, was found to be the best option for the resolution of chlorthalidone enantiomers. Under such conditions, linear calibration curves were obtained in the 0.5-20-microg/ml interval using UV detection at 230 nm. The limit of detection for both isomers was 50 ng/ml. The utility of the described assay has been tested by analyzing chlorthalidone in different pharmaceutical preparations. Examples of application to biological samples are also given.

https://doi.org/10.1016/s0378-4347(00)00103-1