A new, rapid and sensitive spectrophotometric procedure was developed for the estimation of mesalazine (Mesa) in its pharmaceutical forms (PENTASA500 mg). The procedure relies on nitrifying the drug in the presence of acidic conditions with nitrite to generate a diazonium salt, after that adding sulfamic acid to remove the remaining nitrite and then coupling it with a Schiff base to give A yellow dye dissolved in ethanol, and its absorbance was measured against the blank solution at 450nm. The optimum conditions for formation of the product were studied (effect of acid, effect of nitrite amount and time, removal of residual nitrite, effect of Schiff base amount, base size effect, dye stability study). The concentrations obey Beer’s law for the compound ranged from (0.1-2.8) µg/ml, Sandel’s significance was 0. 00502 µg.cm-2, The coefficient was 3.0504 x 104 L.mol-1.cm-1, the LOD was 0. 0017436 µg.ml-1, the LOQ was 0. 00528360 µg.ml-1, and Rec percentage was (99.2708-0102.400) %, RSD% does not exceed 0. 3524 ≥ The method was successfully applied to estimate the (Mesa) in its pharmaceutical preparations by the direct method and the method of single standard additives.

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