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Amino acid based ionic liquids with different proteinogenic l-amino acids were prepared and tested as background electrolyte additives for the separation of phenethylamine enantiomers.A design of experiments approach was performed for the optimization of buffer pH and ionic liquid concentration.Best separations were achieved using tetrabutylammonium l-argininate in a phosphate buffer containing β-cyclodextrin.A synergistic effect between β-CD and l-Arg on the separation of phenethylamine enantiomers was observed.In recent years increasing interest was drawn towards ionic liquids in analytical separation science, such as capillary electrophoresis. Ionic liquids combining tetrabutylammonium cations with chiral amino acid based anions were prepared and investigated as capillary electrophoresis background electrolyte additives for the enantioseparation of ephedrine, pseudoephedrine, and methylephedrine isomers. For the optimization of buffer pH and ionic liquid concentration a design of experiments approach was performed. The best results for the separation of all enantiomers were achieved using 125 mmol/L tetrabutylammonium l-argininate in a 75 mmol/L phosphate buffer pH 1.5 containing 30 mmol/L β-cyclodextrin.