Universität zu Köln

Tretzel, Laura, Thomas, Andreas ORCID: 0000-0003-1199-0743, Geyer, Hans, Delahaut, Philippe, Schaenzer, Wilhelm and Thevis, Mario (2015). Determination of Synacthen(A (R)) in dried blood spots for doping control analysis using liquid chromatography tandem mass spectrometry. Anal. Bioanal. Chem., 407 (16). S. 4709 - 4721. HEIDELBERG: SPRINGER HEIDELBERG. ISSN 1618-2650

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Abstract

Dried blood spot (DBS) sampling, a technique used for taking whole blood samples dried on a filter paper, was initially reported in 1963 by Robert Guthrie. While the diagnostic analysis of metabolic disorders in newborns was the focus of investigations at that time, the number of established applications for preclinical drug development, toxicological studies, and therapeutic drug monitoring increased enormously in the last decades. As a consequence of speed, simplicity, and minimal invasiveness, DBS recommends itself as the preferential technique in sports drug testing. The present approach highlights for the first time the development of a screening assay for the analysis of the synthetic human adrenocorticotropic hormone tetracosactide hexaacetate (Synacthen(A (R))) in DBS using liquid chromatography tandem mass spectrometry. Highly purified sample extracts were obtained by an advanced sample preparation procedure including the addition of an internal standard (d(8)-tetracosactide) and immunoaffinity purification. The method's overall recovery was 27.6 %, and the assay's imprecision was calculated between 8.1 and 17.9 % for intraday and 12.9 to 20.5 % for interday measurements. Stability of the synthetic peptide in DBS was shown for at least 10 days at room temperature and presents a major benefit, since a rapid degradation in conventionally applied matrices such as urine or plasma is well known. With a limit of detection of 50 pg/mL, a detection window of several hours is expected considering reported steady-state plasma levels of 300 pg/mL after intramuscular application of Synacthen(A (R)) Depot (1 mg). The analysis of authentic DBS samples within the scope of an administration study with 250 mu g Synacthen(A (R)) (short stimulation test) demonstrated the great potential of the developed assay to simplify the analysis of Synacthen(A (R)) for doping control purposes.

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Tretzel, Laura UNSPECIFIED UNSPECIFIED UNSPECIFIED Thomas, Andreas UNSPECIFIED orcid.org/0000-0003-1199-0743 UNSPECIFIED Geyer, Hans UNSPECIFIED UNSPECIFIED UNSPECIFIED Delahaut, Philippe UNSPECIFIED UNSPECIFIED UNSPECIFIED Schaenzer, Wilhelm UNSPECIFIED UNSPECIFIED UNSPECIFIED Thevis, Mario UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-402843
DOI:	10.1007/s00216-015-8674-6
Journal or Publication Title:	Anal. Bioanal. Chem.
Volume:	407
Number:	16
Page Range:	S. 4709 - 4721
Date:	2015
Publisher:	SPRINGER HEIDELBERG
Place of Publication:	HEIDELBERG
ISSN:	1618-2650
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language IMMUNOAFFINITY PURIFICATION; LC-MS/MS; PEPTIDES; ACTH; DBS; QUANTIFICATION; PERFORMANCE; VALIDATION; SULFOXIDES; REDUCTION Multiple languages Biochemical Research Methods; Chemistry, Analytical Multiple languages
URI:	http://kups.ub.uni-koeln.de/id/eprint/40284