In this work, a new method has been proposed to simultaneously determine V(V), Co(II) and Cu(II) ions from aqueous solution by spectrophotometry after cloud point extraction using partial least squares regression (PLS). The metal ions in 10 ml of aqueous solution (containing 0.2 M sodium acetate buffer solution, pH 3.5) were formed complexes with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP). Then, Triton X-114 (2 %, v/v) was added to the solution. By increasing the temperature of the solution up to 55 °C, a phase separation occur...