Solid phase extraction (SPE) for the treatment of bovine urine samples in the analysis of β2-agonist multi-residues by gas chromatography-mass spectrometry (GC-MS) was evaluated. Mabuterol, mapenterol, clenproperol, terbutaline, clenbuterol, salbutamol, clenpenterol, bromobuterol and hidroxi-metilclenbuterol (NA1141) were tested with five different mechanisms: adsorption, reverse phase, polar, ion exchange, and mixed phase, and eleven sorbents: diatomaceous earth, octadecyl (C18), octyl (C8), native silica (Si), diol (2OH), amine (NH2), trimethylaminopropyl (SAX), propylbenzenesulphonic (SCX), Bond Elut Certify® (C8+SCX), Clean Screen DAU® (CSDAU) and Multimode (C18+SCX+SAX).