SOLID PHASE EXTRACTION (SPE) FOR MULTI-RESIDUE ANALYSIS OF β2-AGONISTS IN BOVINE URINE

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Abstract
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). Recoveries of the nine β2-agonists from urine samples spiked at 20 ng mL−1 using metoprolol as internal standard were in ranges of 2.9% to 58.1%, of 12.0% to 60.7%, of 6.3% to 31.3%, of 3.3% to 56.8% and of 17.7% to 66.9%, respectively for adsorption, non polar, polar, ion exchange, and multiple extraction mechanisms. The coefficients of variation (C.V.) were also evaluated and discussed. The proposed study show that mixed phase sorbents, especially those which combine hydrophobic and strong cationic exchange interactions, were recommended for a β2-agonist multi-residue solid phase extraction procedure from bovine urine.

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