Identification of an unknown β-agonist in feed by liquid chromatography/bioassay/quadrupole time-of-flight tandem mass spectrometry with accurate mass measurement

• Published in: Rapid communications in mass spectrometry Vol. 17; no. 14; pp. 1633 - 1641
• Main Authors: Nielen, M. W. F., Elliott, C. T., Boyd, S. A., Courtheyn, D., Essers, M. L., Hooijerink, H. H., Bennekom, E. O. van, Fuchs, R. E. M.
• Format: Journal Article
• Language: English
• Published: Chichester, UK John Wiley & Sons, Ltd 01.01.2003
• Subjects: Adrenergic beta-Agonists - analysis; Animal Feed - analysis; chromatography; Chromatography, Liquid; clenbuterol; extraction; Immunoenzyme Techniques; online; Radioligand Assay; Spectrometry, Mass, Electrospray Ionization; urine
• ISSN: 0951-4198; 1097-0231
• DOI: 10.1002/rcm.1099

A new approach to the search for residues of unknown growth promoting agents such as anabolic steroids and β‐agonists in feed is presented. Following primary extraction and clean‐up, samples are separated using gradient liquid chromatography (LC). The effluent is split towards two identical 96‐well fraction collectors and an optional electrospray quadrupole time‐of‐flight mass spectrometry (QTOFMS) system for accurate mass measurement. One 96‐well plate is used for a bioassay (enzyme‐immuno assay, receptor assay) and will detect the bioactivity and position of the relevant peak in the chromatogram. The positive well in the second 96‐well plate is used for identification by LC/QTOFMS/MS. The value of this LC/bioassay/QTOFMS/MS methodology is highlighted by the finding and structure elucidation of a new β‐agonist in a feed extract. Copyright © 2003 John Wiley & Sons, Ltd.