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

• Published in: Journal of liquid chromatography & related technologies Vol. 22; no. 15; pp. 2307 - 2320
• Main Authors: Ramos, Fernando, Bañobre, Maria Carmen, Castilho, Maria da Conceição, da Silveira, Maria Irene Noronha
• Format: Journal Article
• Language: English
• Published: Colchester Taylor & Francis Group 01.01.1999; Taylor & Francis
• Subjects: Animal productions; Biological and medical sciences; Fundamental and applied biological sciences. Psychology; Terrestrial animal productions; Vertebrates; Solid phase extraction; Biological fluid; Agonist; Chemical analysis; Silylation; β2-Adrenergic receptor; β-Adrenergic receptor agonist; Derivatization; Veterinary medicine; Sample preparation; Adsorbent; Ungulata; Electron impact; Urine; Aminoalcohol; Bovine; Coupled method; Benzene derivatives; Gas chromatography; Vertebrata; Mammalia; Multicomponent analysis; Analysis method; Simultaneous measurement; Artiodactyla; Mass spectrometry
• ISSN: 1082-6076; 1520-572X
• DOI: 10.1081/JLC-100101803

Solid phase extraction (SPE) for the treatment of bovine urine samples in the analysis of β 2 -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 (C 18 ), octyl (C 8 ), native silica (Si), diol (2OH), amine (NH 2 ), trimethylaminopropyl (SAX), propylbenzenesulphonic (SCX), Bond Elut Certify® (C 8 +SCX), Clean Screen DAU® (CSDAU) and Multimode (C 18 +SCX+SAX). Recoveries of the nine β 2 -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 β 2 -agonist multi-residue solid phase extraction procedure from bovine urine.