Reliable electrochemical methods, such as cyclic voltammetry, and differential pulse voltammetry techniques were used for the determination of tert-buthylhydroquinone. Metal-organic framework structures with unique superior properties were synthesized. These structures were than combined with methylene blue, an organic dye, to develop an electrochemical sensor for the toxic substance tert-buthylhydroquinone. The electrodes were modified by coating the metal-organic framework-methylene blue composite structure on a glassy carbon electrode and electrochemical determination of tert-buthylhydroquinone was performed. As a result of the study, the amount of the toxic substance was determined sensitively in the linear range 0.1 µM and 2500 µM accurately and rapidly. Characterizations of the obtained materials were performed using different techniques such as UV-Vis, fluorescence spectroscopy, FT-IR, FESEM-EDS, XRD and XPS. After optimizing the conditions, the limit of detection for tert-buthylhydroquinone was 0.05 µM. Additionally, the ratiometric sensor’s usability was evaluated on edible oil samples, resulting in an excellent tert-buthylhydroquinone recovery between 98.50% and 102.40%.