Sensitive hydrophilic interaction liquid chromatography/tandem mass spectrometry method for rapid detection, quantification and confirmation of cathinone-derived designer drugs for doping control in equine plasma
Article first published online: 5 DEC 2013
Copyright © 2013 John Wiley & Sons, Ltd.
Rapid Communications in Mass Spectrometry
Volume 28, Issue 2, pages 217–229, 30 January 2014
How to Cite
Li, X., Uboh, C. E., Soma, L. R., Liu, Y., Guan, F., Aurand, C. R., Bell, D. S., You, Y., Chen, J. and Maylin, G. A. (2014), Sensitive hydrophilic interaction liquid chromatography/tandem mass spectrometry method for rapid detection, quantification and confirmation of cathinone-derived designer drugs for doping control in equine plasma. Rapid Commun. Mass Spectrom., 28: 217–229. doi: 10.1002/rcm.6778
- Issue published online: 5 DEC 2013
- Article first published online: 5 DEC 2013
- Manuscript Accepted: 31 OCT 2013
- Manuscript Revised: 29 OCT 2013
- Manuscript Received: 18 SEP 2013
Cathinone derivatives are new amphetamine-like stimulants that can evade detection when presently available methods are used for doping control. To prevent misuse of these banned substances in racehorses, development of a liquid chromatography/tandem mass spectrometry (LC/MS/MS) method became the impetus for undertaking this study.
Analytes were recovered via liquid-liquid extraction using methyl tert-butyl ether. Analyte separation was achieved on a hydrophilic interaction column using liquid chromatography and mass analysis was performed on a QTRAP mass spectrometer in positive electrospray ionization (ESI) mode with multiple reaction monitoring (MRM). Analyte identification was carried out by screening for a specified MRM transition. Quantification was conducted using an internal standard. Confirmation was performed by establishing a match in retention time and ion intensity ratios comparison.
The method was linear over the range 0.2–50 ng/mL. The specificity was evaluated by analysis of six different batches of blank plasma and those spiked with each analyte (0.2 ng/mL). The recovery of analytes from plasma at three different concentrations was >70%. The limits of detection, quantification and confirmation were 0.02–0.05, 0.2–1.0 and 0.2–10 ng/mL, respectively. The matrix effect was insignificant. The intra-day and inter-day precision were 1.94–12.08 and 2.58–13.32%, respectively.
The method is routinely employed in screening for the eleven analytes in post-competition samples collected from racehorses in Pennsylvania to enforce the ban on the use of these performance-enhancing agents in racehorses. The method is sensitive, fast, effective and reliably reproducible. Copyright © 2013 John Wiley & Sons, Ltd.