This article is part of the Journal of Mass Spectrometry special issue entitled “2nd MS Food Day” edited by Gianluca Giorgi.
Analytical investigations about the presence of prednisolone in cow urine†
Article first published online: 6 SEP 2012
Copyright © 2012 John Wiley & Sons, Ltd.
Journal of Mass Spectrometry
Special Issue: 2nd MS Food Day
Volume 47, Issue 9, pages 1221–1231, September 2012
How to Cite
Dusi, G., Vago, G., Ghidelli, V., Pellegrino, R. M. and Galarini, R. (2012), Analytical investigations about the presence of prednisolone in cow urine. J. Mass Spectrom., 47: 1221–1231. doi: 10.1002/jms.3066
- Issue published online: 6 SEP 2012
- Article first published online: 6 SEP 2012
- Manuscript Accepted: 14 JUL 2012
- Manuscript Revised: 5 JUL 2012
- Manuscript Received: 23 MAR 2012
- high-resolution mass spectrometry;
- Commission Decision 2002/657/EC
Since 2008, the analyses carried out in the Lombardia region as part of National Residue Control Plans have evidenced unexpected frequent detection of the corticosteroid prednisolone (PRED) in cow urine samples taken to the slaughterhouse. Considering the scarce plausibility of these high frequent findings, analytical investigations were started to ascertain the real presence of this corticosteroid. The applied confirmatory method involved liquid-chromatography low-resolution tandem mass spectrometry (triple quadrupole) as instrumental technique, and it was validated in compliance with the requirements of the Commission Decision 2002/657/EC. However, recently some criticism regarding Commission Decision 2002/657/EC identification criteria has been pointed out, experimentally demonstrating false positive results (wrong identification) although these criteria have been strictly observed. Therefore, considering the serious implications (i.e. the possibility that PRED could be considered endogenous in particular animal conditions), studies were carried out to investigate the reliability of PRED identification through the change of the chromatographic conditions (mobile phases, gradient and analytical column) of the confirmatory procedure routinely applied. Further confirmation came from the application of high-resolution mass spectrometry technique (MS2 and MS3 experiments) to analyze incurred cow urines samples. All the obtained results confirmed definitively the real presence of this corticosteroid excluding false-positive findings in routine analysis. In addition, other experiments demonstrated that high-resolution mass spectrometers (Time of Flight and Orbitrap technologies) could be successfully applied to routine determination of steroid residues in biological fluids at very low concentrations (< 1 µg L−1). Copyright © 2012 John Wiley & Sons, Ltd.