Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume
46, Number 2, February 2008, pp. 174-183
Optimization of Solid-Phase Extraction for the
Liquid Chromatography–Mass Spectrometry Analysis of Harpagoside,
8-para-Coumaroyl Harpagide, and Harpagide in Equine Plasma and
Urine
Cyril Colas[1,2], Patrice Garcia[1], Marie-Agnès
Popot[1], Yves Bonnaire[1], and Stéphane Bouchonnet[2]
[1]LCH—Laboratoire des Courses Hippiques, 15 rue de Paradis, 91370
Verrières le Buisson, France; and
[2]DCMR – Laboratoire des
Mécanismes Réactionnels, Département de Chimie, École
Polytechnique, CNRS, route de Saclay, 91128 Palaiseau cedex,
France
Solid-phase extraction cartridges among those
usually used for screening in horse doping analyses are tested
to optimize the extraction of harpagoside (HS), harpagide (HG),
and 8-para-coumaroyl harpagide (8PCHG) from plasma and urine.
Extracts are analyzed by liquid chromatography coupled with multi-step
tandem mass spectrometry. The extraction process retained for
plasma applies BondElut PPL cartridges and provides extraction
recoveries between 91% and 93%, with RSD values between 8 and
13% at 0.5 ng/mL. Two different procedures are needed to extract
analytes from urine. HS and 8PCHG are extracted using AbsElut
Nexus cartridges, with recoveries of 85% and 77%, respectively
(RSD between 7% and 19%). The extraction of HG involves the use
of two cartridges: BondElut PPL and BondElut C18 HF, with recovery
of 75% and RSD between 14% and 19%. The applicability of the
extraction methods is determined on authentic equine plasma and
urine samples after harpagophytum or harpagoside administration.
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