Universität zu Köln

Lange, Tobias, Thomas, Andreas, Walpurgis, Katja and Thevis, Mario (2020). Fully automated dried blood spot sample preparation enables the detection of lower molecular mass peptide and non-peptide doping agents by means of LC-HRMS. Anal. Bioanal. Chem., 412 (15). S. 3765 - 3778. HEIDELBERG: SPRINGER HEIDELBERG. ISSN 1618-2650

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Abstract

The added value of dried blood spot (DBS) samples complementing the information obtained from commonly routine doping control matrices is continuously increasing in sports drug testing. In this project, a robotic-assisted non-destructive hematocrit measurement from dried blood spots by near-infrared spectroscopy followed by a fully automated sample preparation including strong cation exchange solid-phase extraction and evaporation enabled the detection of 46 lower molecular mass (< 2 kDa) peptide and non-peptide drugs and drug candidates by means of LC-HRMS. The target analytes included, amongst others, agonists of the gonadotropin-releasing hormone receptor, the ghrelin receptor, the human growth hormone receptor, and the antidiuretic hormone receptor. Furthermore, several glycine derivatives of growth hormone-releasing peptides (GHRPs), arguably designed to undermine current anti-doping testing approaches, were implemented to the presented detection method. The initial testing assay was validated according to the World Anti-Doping Agency guidelines with estimated LODs between 0.5 and 20 ng/mL. As a proof of concept, authentic post-administration specimens containing GHRP-2 and GHRP-6 were successfully analyzed. Furthermore, DBS obtained from a sampling device operating with microneedles for blood collection from the upper arm were analyzed and the matrix was cross-validated for selected parameters. The introduction of the hematocrit measurement method can be of great value for doping analysis as it allows for quantitative DBS applications by managing the well-recognized hematocrit effect. Graphical abstract

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Lange, Tobias UNSPECIFIED UNSPECIFIED UNSPECIFIED Thomas, Andreas UNSPECIFIED UNSPECIFIED UNSPECIFIED Walpurgis, Katja UNSPECIFIED UNSPECIFIED UNSPECIFIED Thevis, Mario UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-332403
DOI:	10.1007/s00216-020-02634-4
Journal or Publication Title:	Anal. Bioanal. Chem.
Volume:	412
Number:	15
Page Range:	S. 3765 - 3778
Date:	2020
Publisher:	SPRINGER HEIDELBERG
Place of Publication:	HEIDELBERG
ISSN:	1618-2650
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language HORMONE-RELEASING PEPTIDE-2; HUMAN URINE; LIQUID-CHROMATOGRAPHY; HEMATOCRIT; GHRP-2; IDENTIFICATION; METABOLITES Multiple languages Biochemical Research Methods; Chemistry, Analytical Multiple languages
URI:	http://kups.ub.uni-koeln.de/id/eprint/33240