Part I. Rapid analysis of pharmaceutical compounds using high-speed HPLC columns. Part II. Simulataneous determination of drugs in tablet dosage forms using packed column supercritical fluid chromatography. Part III. Pharmaceutical analysis of selected

Part I of this dissertation describes the use of high speed HPLC columns: Alltech Rocket Alltima C 18, Micra NPS ODS-I, and HP Zorbax SB-C18, for separations of selected drug mixtures. The high speed resolution without loss of efficiency resulted from the use of short column lengths and small-size particles.; In Chapter I, two drug combinations, codeine-guaifenesin and acetaminophen-caffeine, were investigated on three high speed columns. Baseline separations were achieved with all columns under 4 min. Intra- and inter-day RSD, limits of detection, retention factors, theoretical plates, tailing factors, selectivity values, and resolutions were calculated for the separated drugs.; In Chapter II, methods are presented using high speed columns for three selected analyte mixtures, theophylline-guaifenesin, acetaminophen-codeine, and hydrochlorothiazide-propranolol. The performance of each column was compared by studying different chromatographic parameters.; In Part II of this dissertation, packed column supercritical fluid chromatography (SFC) is used in the various applications of pharmaceutical analysis.; Chapter III describes an isobaric and isothermal separation of a trimethoprim and sulfamethoxazole mixture using packed column SFC.; In Chapter IV, a SFC separation method for a chlordiazepoxide and amitriptyline mixture is described. Part III of this dissertation presents pharmaceutical analysis applications of selected drugs using capillary electrophoresis (CE).; In Chapter V, a micellar electrokinetic capillary chromatography (MEKC) method was developed for the simultaneous determination of a trimethoprim and sulfamethoxazole mixture in bulk and tablet dosage forms.; In Chapter VI, an amitriptyline and chlordiazepoxide mixture was quantified in bulk and tablet dosage forms by a capillary zone electrophoresis (CZE) method.; In Chapter VII, the D and L enantiomers of vesamicol were resolved using sulfated-β-cyclodextrin (S-β-CD) in CE. The effects of various factors such as cyclodextrin (CD) type, CD concentration, buffer type, buffer concentration, and pH on the enantioseparations were investigated.; In Chapter VIII, a chiral CE method for nomifensine, a dopamine uptake blocker, in human serum samples is described. The Bond Elut C 18 cartridges were used for solid phase extraction (SPE) of nomifensine serum samples with absolute recoveries in excess of 95% for the enantiomers. The limits of detection (LODs) (S/N = 3) were 0.5 μg/ml for both enantiomers at 210 nm. Calibration curves were obtained using an internal standard method with regression coefficients greater than 0.991 (n = 15).