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In this research work a simple and very fast salting-out assisted liquid–liquid extraction (SALLE) followed by UV–vis spectrphotometric method was developed and applied for determination of methylene blue and sunset yellow in wastewater and food samples. Water-miscible extraction solvent (4.5mL acetonitrile) was added to aqueous solution (5.5mL) for formation of a homogeneous solution. To the mixture solution, suitable amount of (NH₄)₂SO₄ was added, the mixture solution was shaken until the salt was dissolved, and then it was separated into two clear phases easily and rapidly. The target analytes in the sample was extracted into the water-miscible extraction solvent. After extraction, the analytes in the organic phase was determined by spectrphotometric method using the analytical wavelengths of 417nm, 656nm for sunset yellow and methylene blue, respectively. The influences of effective parameters …