This thesis exemplifies an analytical quantification for some drugs acting as cardiovascular agents; namely Clopidogrel bisulphate (CPS), Aspirin (ASP), Simvastatin (SMT), Atenolol (ATN), Ramipril (RAM), Hydrochlorothiazide (HCTZ), Telmisartan (TEL), and Chlorthalidone (CLT), together with the anti-infective agent Amprolium hydrochloride (AMP). The goal of this thesis was to develop and utilize sensitive, accurate and selective analytical methods capable of quantitative analysis of the above-mentioned drugs in their mixtures. The proposed methods were also tuned to determine the analyte of interest in its pharmaceutical dosage form and in biological fluids, furthermore, results from the proposed methods were statistically compared with those of pharmacopeial or reported method.