A master's dissertation was discussed in the College of Science, Al-Nahrain University on studying the properties of the new selective ionic electrodes of afloxacin and norfloxacin and comparing them with high performance liquid chromatography by the postgraduate student, Mrs. Suad Jawad Abid. The dissertation aimed at finding a new analytical method for estimating the two drugs afloxacin and norfloxacin in pharmaceutical preparations and human fluids (serum and urine) and comparing them with standard methods of high-performance liquid chromatography. The dissertation reviewed preparing six ionic selective electrodes based on combining the two drugs with a reagent (methyl orange) via using three types of plasticizers, dibutyl phthalate, ethylhexyl phosphate and dibutyl sibacate. The dissertation concluded that giving the electrodes to both afloxacin and norfloxacin and with the plasticizer will give the best results when compared with the HPLC method, as it was found that there is no fundamental difference in terms of accuracy and compatibility.