Universität zu Köln

Goergens, Christian, Guddat, Sven, Orlovius, Anne-Katrin, Sigmund, Gerd, Thomas, Andreas ORCID: 0000-0003-1199-0743, Thevis, Mario and Schaenzer, Wilhelm (2015). Dilute-and-inject multi-target screening assay for highly polar doping agents using hydrophilic interaction liquid chromatography high resolution/high accuracy mass spectrometry for sports drug testing. Anal. Bioanal. Chem., 407 (18). S. 5365 - 5380. HEIDELBERG: SPRINGER HEIDELBERG. ISSN 1618-2650

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Abstract

In the field of LC-MS, reversed phase liquid chromatography is the predominant method of choice for the separation of prohibited substances from various classes in sports drug testing. However, highly polar and charged compounds still represent a challenging task in liquid chromatography due to their difficult chromatographic behavior using reversed phase materials. A very promising approach for the separation of hydrophilic compounds is hydrophilic interaction liquid chromatography (HILIC). Despite its great potential and versatile advantages for the separation of highly polar compounds, HILIC is up to now not very common in doping analysis, although most manufacturers offer a variety of HILIC columns in their portfolio. In this study, a novel multi-target approach based on HILIC high resolution/high accuracy mass spectrometry is presented to screen for various polar stimulants, stimulant sulfo-conjugates, glycerol, AICAR, ethyl glucuronide, morphine-3-glucuronide, and myo-inositol trispyrophosphate after direct injection of diluted urine specimens. The usage of an effective online sample cleanup and a zwitterionic HILIC analytical column in combination with a new generation Hybrid Quadrupol-OrbitrapA (R) mass spectrometer enabled the detection of highly polar analytes without any time-consuming hydrolysis or further purification steps, far below the required detection limits. The methodology was fully validated for qualitative and quantitative (AICAR, glycerol) purposes considering the parameters specificity; robustness (rRT < 2.0 %); linearity (R > 0.99); intra- and inter-day precision at low, medium, and high concentration levels (CV < 20 %); limit of detection (stimulants and stimulant sulfo-conjugates < 10 ng/mL; norfenefrine; octopamine < 30 ng/mL; AICAR < 10 ng/mL; glycerol 100 mu g/mL; ETG < 100 ng/mL); accuracy (AICAR 103.8-105.5 %, glycerol 85.1-98.3 % at three concentration levels) and ion suppression/enhancement effects.

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Goergens, Christian UNSPECIFIED UNSPECIFIED UNSPECIFIED Guddat, Sven UNSPECIFIED UNSPECIFIED UNSPECIFIED Orlovius, Anne-Katrin UNSPECIFIED UNSPECIFIED UNSPECIFIED Sigmund, Gerd UNSPECIFIED UNSPECIFIED UNSPECIFIED Thomas, Andreas UNSPECIFIED orcid.org/0000-0003-1199-0743 UNSPECIFIED Thevis, Mario UNSPECIFIED UNSPECIFIED UNSPECIFIED Schaenzer, Wilhelm UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-399847
DOI:	10.1007/s00216-015-8699-x
Journal or Publication Title:	Anal. Bioanal. Chem.
Volume:	407
Number:	18
Page Range:	S. 5365 - 5380
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 URINARY-EXCRETION; MYOINOSITOL TRISPYROPHOSPHATE; PHYSIOLOGICAL DISPOSITION; P-HYDROXYMETHAMPHETAMINE; ALLOSTERIC EFFECTOR; REVERSED-PHASE; METABOLITES; METHAMPHETAMINE; GLUCURONIDE; SEPARATION Multiple languages Biochemical Research Methods; Chemistry, Analytical Multiple languages
URI:	http://kups.ub.uni-koeln.de/id/eprint/39984