Chromatographic techniques, such as high performance liquid chromatography (HPLC) and ion chromatography (IC), have traditionally been employed in the analysis of a variety of analytes, such as inorganic anions, organic acids and pharmaceuticals. Capillary electrophoresis (CE) methods have recently been developed for their determination and can be ideal methods due to low sample and material consumption, reduced analysis times and increased separation efficiencies. A HPLC method was developed and successfully applied to the analysis of the photoinitiator, bis(2,4,6-trimethylbenzoyl)phenyl-phosphine oxide. A comparison of its stability in samples, which were both kept in the dark and exposed to the light, was performed using the optimised HPLC-UV method. From this it was determined that complete degradation of the Irgacure had occurred by 60 min. for the samples exposed to the light. The curing mechanism of the Irgacure was determined using HPLC-MS, and it was determined that the Irgacure undergoes a free radical cunhg reaction. There are a wide range of inorganic and acidic anions that may be present at different stages of the cyanoacrylate adhesive production process. A highly efficient CE separation was developed and applied to the simultaneous determination of inorganic and acidic anions, which are present in ethyl cyanoacrylate adhesive samples. The CE method developed was compared with IC, the method traditionally employed for their analysis. CE offers advantages over the IC method, namely reduced sample volumes and waste and also more rapid separation. From this investigation, CE was demonstrated to bc an effective method for their quantification, as it enabled the sensitive monitoring of the cyanoacrylate production process. A CE method was developed for the simultaneous analysis of the anthracyclines, daunombicin, doxorubicin and epirubicin. Ultra-violet (UV), electrochemical (EC) and laser-induced fluorescence (LIF) detection coupled to CE were investigated. Improved detection limits (150-1400 ng ml-') were obtained with LIF detection, which were capable of monitoring the therapeutic levels (5-50,000 ng ml-') of anthracyclines. For the real time monitoring of anthracyclines in plasma, it was preferred that minimal sample pre-treatment was carried out. The feasibility of analysing plasma samples without sample pre-treatment was demonstrated. The degree of plasma protein binding of anthracyclines was determined using microdialysis, and the potential of this technique for the real time monitoring of plasma samples with on-line microdialysis coupled with CE was demonstrated. Microdialysis is suitable for coupling to CE as it generates sample volumes that are ideal for CE.