The corrosion product deposit (crud) found on the surface of the fuel rod of the pressurized water reactors (PWRs) chiefly made up of nickel ferrite. Fe, Co, Ni and Cr are the major elements exist in PWR crud. Ascribable to the simplicity in execution, handling, and option for recyclability, solvent extraction technique has been broadly used in nuclear energy sector. In the present investigation, the recovery of iron, cobalt, and nickel has been studied from simulated crud solution in nitrate medium using a novel hydrophobic menthol‐decanoic acid‐based deep eutectic solvent. Process parameters such as pH, DES concentration and shaking time were considered as input variables, and concentration of Fe, Co, and Ni as response variables for the design of experiments. Response surface methodology via Box‐Behnken design using polynomial quadratic model was selected for optimization of solvent extraction experiments. A total of 17 runs were conducted and the results were used for optimization purpose. Complete separation of Co/Fe and Co/Ni is achievable under various extraction conditions. As per the BBD analysis, the optimization conditions obtained were pH=1.9, [DES]=2.99 mol/L and shaking duration=18.27 min. Under these conditions,the amount of Fe, Co and Ni extracted were found as 32.29 g/L, 0.2111 g/L, and 19.83 g/L, respectively.