ABSTRACT The studies presented in this work include novel analytical methods based on spectrofluorimetric techniques for determination of some organic compounds used in pharmaceutical preparations. The work is divided to three chapters. The first chapter includes general introduction of spectrofluorimetric activity of lanthanide elements and the parameters affects on these phenomena. Also, the chapter involved the review of literature for previous methods of metoclopramide and hydrochlorothiazide drugs determination. The second chapter deals with the materials and apparatus used during this work including the types, grades, sources and preparations of these materials. Also, include the methods for measurements of different factors as absorbance, excitation and emission, effect of pH, effect of reagents and the validity tests of the metoclopramide and hydrochlorothiazide proposed methods as selectivity, recovery, precision and stability. The third chapter includes the results and discussion of the proposed methods for determination of metoclopramide hydrochloride (MCP) and hydrochlorothiazide (HCT).