The research presented in this thesis has centered on the development of newer and better techniques for the determination of coumann, 7-hydroxycoumann and 7-hydroxycoumannglucuromde. The methods developed were applied to clinical studies of biological fluids including serum, plasma and urine and after in vitro metabolism of coumann and 7- hydroxycoumann. The techniques employed include capillary electrophoresis (CE), highperformance liquid chromatography (HPLC) and antibody-based immunoanalytical techniques. A separation based on capillary electrophoresis (CE) was developed for determining free and total 7-hydroxycoumann in serum and unne after the in vivo metabolism of coumann The compound was extracted into ether, evaporated to dryness and reconstituted into phosphate buffer before analysis by CE. The separation method developed was then applied to the determination of 7-hydroxycoumann, without sample clean-up, after in vitro metabolism of coumann by liver microsomal suspensions. The inter-species and inter-individual variation in coumann metabolism was assessed. A large variation within species (human microsomal preparations - n = 5) and between species (n = 10) was found Another CE method was developed for the direct determination of free 7-hydroxycoumann and conjugated 7- hydroxycoumann in unne after in vivo metabolism of coumann. This method was also applied to the determination of 7-hydroxycoumann-glucuronide after in vitro metabolism of 7-hydroxycoumann by undine diphosphate glucuronyl transferase in a crude enzymatic preparation from liver. High-performance liquid chromatography was used for the determination of coumann, 7- hydroxycoumann and 7-hydroxycoumann-glucuronide in unne, plasma and serum. An isocratic separation method was utilised for the determination of total 7-hydroxycoumann after the administration of 7-hydroxycoumann to patients diagnosed with a range of cancers. The method was used to determine the pharmacokinetic profile of serum levels of the drug. A range of 7-hydroxycoumann doses were given (100 mg - 7000 mg) and the mtenndividual variations in 7-hydroxycoumann metabolism were determined Separations were based on enzymatic deconjugation of 7-hydroxycoumann from the glucuromde form, followed by extraction into ether, evaporation to dryness, and reconstitution into methanol before analysis by HPLC A gradient separation method was also developed for the direct determination of coumann, 7-hydroxycoumann, and 7-hydroxycoumann-glucuromde in urine, plasma and serum after the in vivo metabolism of coumann and 7-hydroxycoumann. The method was also used for the determination of 7-hydroxycoumann-glucuromde after the in vitro metabolism of 7-hydroxycoumann by a crude enzymatic preparation from liver. A 7-hydroxycoumann-thyroglobuhn protem-drug conjugate was prepared. It was used in the generation of rabbit polyclonal antibodies Antibodies raised against the protein-drug conjugate were screened against another protein-drug conjugate (bovine serum albuimn-7- hydroxycoumann) to determine the antibody titre The antibodies raised were purified from rabbit serum, characterised and utilised in an enzyme-linked immunosorbent assay.