The determination of inorganic mercury species in water, beverages and foods has been a special research priority in recent years because mercury, as a highly carcinogenic species, even in trace concentration, has high adverse effects on the body of living organisms. In this research, combining two extraction techniques, including microwave‐assisted cloud point extraction and dispersive‐solid phase extraction (MA‐CP‐dSPE), for the separation and pre‐concentration of mercury in environmental samples is presented. This method is based on the dispersion of nanoparticles in micellar media in the presence of a novel mono‐thiosemicarbazone Schiff base (2 N′‐[4‐diphenylamino]benzylidene) hydrazinecarbothiohydrazide) ligand. Using the experimental conditions defined in the optimization, the method allowed mercury determination from 0.020 to 350 mg/L with a detection limit of 0.005 mg/L. The accuracy of the procedure was tested by analysing certified reference material. The method was successfully applied to copper determination in spring water, beverage and rice samples.