Determination of Synacthen in human plasma using immunoaffinity purification and liquid chromatography/tandem mass spectrometry

Mario Thevis, Michael Bredehöft, Hans Geyer, Matthias Kamber, Philippe Delahaut, Wilhelm Schänzer

Publikation: Beitrag in FachzeitschriftZeitschriftenaufsätzeForschungBegutachtung

Abstract

Synacthen is a synthetic analogue to human adrenocorticotropin, which plays an important physiological role by stimulating production of cortisol. In sports, corticosteroids as well as releasing factors (corticotropins) are prohibited according to the regulations of the World Anti-Doping Agency, and the misuse of Synacthen has been reported several times. Hence, an assay enabling the detection of Synacthen in doping control samples has been developed using immunoaffinity chromatographic isolation of Synacthen from human plasma combined with a concentration of collected fractions using solid-phase extraction. Unambiguous determination of the target analyte was accomplished using microbore liquid chromatography/electrospray ionization tandem mass spectrometry. Diagnostic product ions such as m/z 223 were characterized using high-resolution/high-accuracy Orbitrap mass spectrometry and employed for triple quadrupole MS/MS analysis. The established assay requiring 2 mL of plasma allowed a lower limit of detection (LLOD) at 100 fmol/mL, a recovery of 97% and a precision at the LLOD < 20%. Authentic plasma samples obtained from a patient undergoing a standard short Synacthen test were used to prove the applicability of the developed procedure.

OriginalspracheEnglisch
ZeitschriftRapid communications in mass spectrometry : RCM
Jahrgang20
Ausgabenummer23
Seiten (von - bis)3551-3556
Seitenumfang6
ISSN0951-4198
DOIs
PublikationsstatusVeröffentlicht - 01.01.2006

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