Part I: Pharmaceutical analysis of selected drugs using HPLC and mass spectrometry. Part II: Pharmaceutical analysis of selected drugs using capillary electrophoresis

Part I of this dissertation describe the application of liquid chromatography-mass spectrometry and nonporous octadecylsilane columns in the analysis of various model drugs.; In Chapter I, the stability of sumatriptan succinate in bulk drug and tablet dosage form was studied. Acid, base, heat and oxidation stressed methods were applied to sumatriptan succinate. Mass spectrometry was used to determine the identity of a number of degradation products from the bulk drug. Liquid chromatography coupled with mass spectrometry was used to analyze the degraded samples and identifications of degradates were made.; Chapter II describes the analysis of ondansetron and its 6-, 7- and 8-hydroxy metabolites in human serum using solid phase extraction (SPE) and positive ionization LC-ESI-MS-MS. Linearity was in the range 1–500 ng/ml for ondansetron and each of the hydroxyl metabolites; Chapters III–V present high performance liquid chromatography (HPLC) procedures using non-porous ODS columns. In Chapter III, a method was developed for the assay of aspirin-caffeine-butalbital and acetaminophen-caffeine-butalbital. In Chapter IV, a fast and sensitive reverse phase HPLC-UV method for the separation and quantitation of haloperidol and its related in both drug substance and tablet dosage form is presented using non-porous silica (NPS) ODS-I column. In Chapter V, a comparison of the current USP ODS chromatographic purity method for vancomycin to a nonporous ODS method was performed.; In Part II of this dissertation, capillary electrophoresis method development and validation for bulk drug and drugs in serum is presented.; Chapter VI illustrates an assay for dopamine D-2 receptor antagonists eticlopride and sulpiride in serum using capillary electrophoresis with cyclodextrin additives. Chiral resolution of S(−) and R(+) sulpiride and eticlopride were achieved using 2% sulfated-β-cyclodextrin (S-β-CD) in 20 mM citrate run buffer (pH 2.90). The reversed polarity mode voltage of 20 kV was used for the analysis. Calibration curves, precision and accuracy of the method were also presented.; In Chapter VII, a MEKC method for the simultaneous determination of guaifenesin, pseudoephedrine and dextromethorphan in a capsule dosage form is described. Coefficients of determination were greater than 0.9989 (n = 12). Precision and accuracy of the method were better than 7%.