AUTOMATED-ANALYSIS OF A NOVEL ANTIEPILEPTIC COMPOUND, CGP-33-101, ANDITS METABOLITE, CGP-47-292, IN BODY-FLUIDS BY HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY AND LIQUID-SOLID EXTRACTION

Automated procedures for the determination of CGP 33 101 in plasma and the simultaneous determination of CGP 33 101 and its carboxylic acid metabolite, CGP 47 292, in urine are described. Plasma was diluted wit h water and urine with a pH 2 buffer prior to extraction. The compound s were automatically extracted on reversed-phase extraction columns an d injected onto an HPLC system by the automatic sample preparation wit h extraction columns (ASPEC) automate. A Supelcosil LC-18 (5 mu m) col umn was used for chromatography. The mobile phase was a mixture of an aqueous solution of potassium dihydrogen phosphate, acetonitrile and m ethanol for the assay in plasma, and of an aqueous solution of tetrabu tylammonium hydrogen sulfate, tripotassium phosphate and phosphoric ac id and of acetonitrile for the assay in urine. The compounds were dete cted at 230 nm. The limit of quantitation was 0.11 mu mol/l (25 ng/ml) for the assay of CGP 33 101 in plasma, 11 mu mol/l (2.5 mu g/ml) for its assay in urine and 21 mu mol/l (5 mu g/ml) for the assay of CGP 47 292 in urine.