Enzymatic alcoholysis of fish oil can produce monoacylglycerols rich in polyunsaturated fatty acids at atmospheric pressure and low temperature. Biocatalysis in organic solvents helps to create a homogeneous reaction system for the reactants, ethanol and fish oil. This work presents liquid liquid equilibrium at two different temperatures (303.2 K and 323.2 K) and at atmospheric pressure for two solvent-systems in the ethanolysis of fish oil: ethanol + oil + tert-pentanol and ethanol + oil + hexane. Experimental solubility (binodal) curves were obtained by the cloud point method and tie-line composition was obtained by density and high-temperature gas chromatography. The consistency of experimental tie-line data was checked by using the Othmer-Tobias equation. The experimental liquid-liquid data were correlated satisfactorily by the nonrandom two liquid model for activity coefficient calculations.