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Abstract This thesis is concerned with the analysis of some pharmaceutical compounds in different mixtures. It comprises three parts, part I is about determination of acefylline piperazine and bromhexine hydrochloride in the presence of their degradation products and dosage form excipients (methyl and propylparabens). While part II is about the simultaneous analysis of a binary mixture of camylofin dihyrochloride and analgin in the presence of their degradation products. In addition to Part III which is concerned with the simultaneous analysis of a binary mixture of calcipotriol monohydrate and betamethasone dipropionate in the presences of dosage form excipients (butylated hydroxytoluene and alpha-tocopherol). Various analytical techniques were used for the simultaneous analysis of these mixtures. The applied techniques include spectrophotometry, chemmometry, thin layer chromatography (TLC), high performance liquid chromatography (HPLC) and electrochemistry. The proposed methods were simple, accurate, and reproducible, which would be feasible, and sensitive for the determination of the studied drugs. The proposed methods were validated according to ICH-guidelines |