Universität zu Köln

Thomas, A., Solymos, E., Schaenzer, W., Baume, N., Saugy, M., Dellanna, F. and Thevis, M. (2011). Determination of Vasopressin and Desmopressin in urine by means of liquid chromatography coupled to quadrupole time-of-flight mass spectrometry for doping control purposes. Anal. Chim. Acta, 707 (1). S. 107 - 114. AMSTERDAM: ELSEVIER SCIENCE BV. ISSN 1873-4324

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Abstract

The anti-diuretic neurohypophysial hormone Vasopressin (Vp) and its synthetic analogue Desmopressin (Dp. 1-desamino-vasopressin) have received considerable attention from doping control authorities due to their impact on physiological blood parameters. Accordingly, the illicit use of Desmopressin in elite sport is sanctioned by the World Anti-Doping Agency (WADA) and the drug is classified as masking agent. Vp and Dp are small (8-9 amino acids) peptides administered orally as well as intranasally. Within the present study a method to determine Dp and Vp in urinary doping control samples by means of liquid chromatography coupled to quadrupole high resolution time-of-night mass spectrometry was developed. After addition of Lys-Vasopressin as internal standard and efficient sample clean up with a mixed mode solid phase extraction (weak cation exchange), the samples were directly injected into the LC-MS system. The method was validated considering the parameters specificity, linearity, recovery (80-100%), accuracy, robustness, limit of detection/quantification (20/50 pg mL(-1)), precision (inter/intraday < 10%), ion suppression and stability. The analysis of administration study urine samples collected after a single intranasal or oral application of Dp yielded in detection windows for the unchanged target analyte for up to 20 h at concentrations between 50 and 600 pg mL(-1). Endogenous Vp was detected in concentrations of approximately 20-200 pg mL(-1) in spontaneous urine samples obtained from healthy volunteers. The general requirements of the developed method provide the characteristics for an easy transfer to other anti-doping laboratories and support closing another potential gap for cheating athletes. (C) 2011 Elsevier B.V. All rights reserved.

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Thomas, A. UNSPECIFIED UNSPECIFIED UNSPECIFIED Solymos, E. UNSPECIFIED UNSPECIFIED UNSPECIFIED Schaenzer, W. UNSPECIFIED UNSPECIFIED UNSPECIFIED Baume, N. UNSPECIFIED UNSPECIFIED UNSPECIFIED Saugy, M. UNSPECIFIED UNSPECIFIED UNSPECIFIED Dellanna, F. UNSPECIFIED UNSPECIFIED UNSPECIFIED Thevis, M. UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-485081
DOI:	10.1016/j.aca.2011.09.027
Journal or Publication Title:	Anal. Chim. Acta
Volume:	707
Number:	1
Page Range:	S. 107 - 114
Date:	2011
Publisher:	ELSEVIER SCIENCE BV
Place of Publication:	AMSTERDAM
ISSN:	1873-4324
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language 1-DEAMINO-8-D-ARGININE VASOPRESSIN; PLASMA-CONCENTRATIONS; PHARMACOKINETICS; OXYTOCIN; PHARMACODYNAMICS; METABOLISM; PROTEINS; SPECTRA; ANALOGS; DDAVP Multiple languages Chemistry, Analytical Multiple languages
URI:	http://kups.ub.uni-koeln.de/id/eprint/48508