Universität zu Köln

Mehling, Lena-Maria, Piper, Thomas ORCID: 0000-0002-7462-6693, Dib, Josef, Pedersen, Daniel Sejer ORCID: 0000-0003-3926-7047, Madea, Burkhard, Hess, Cornelius and Thevis, Mario (2017). Development and validation of a HPLC-QTOF-MS method for the determination of GHB-beta-O-glucuronide and GHB-4-sulfate in plasma and urine. Forensic Toxicol., 35 (1). S. 77 - 86. NEW YORK: SPRINGER. ISSN 1860-8973

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Abstract

Gamma-hydroxybutyric acid (GHB) is used as a so-called knock-out drug in drug-facilitated sexual assault. Due to GHB's short detection window in blood and urine, crime verification remains problematic in many cases. Phase II metabolites can enhance the detectability and prolong the detection window of some lower-molecular-mass molecules, as exemplified by ethanol. GHB-beta-O-glucuronide (GHB-Gluc) was recently introduced as one phase II metabolite, and GHB-4-sulfate (GHB-Sulf) was also postulated to represent a urinary metabolite of exogenous GHB. To unambiguously verify the presence of GHB-Sulf in urine, the reference standard material of GHB-Sulf was synthesized, together with its deuterated analogue, GHB-Sulf-d (6). This reference standard material, together with GHB-Gluc and GHB-Gluc-d (4), was employed to develop and validate a quantitative method for determining both target analytes in plasma and urine samples. Compounds were separated by high-performance liquid chromatography on a Hypercarb column and detected by electrospray ionization time-of-flight-mass spectrometry. Calibration curves were linear over the entire calibration range up to 20 mg/L, and quantification limits of < 0.01 mg/L were achieved. Accuracy and interday and intraday precision fulfilled all forensic guidelines criteria. In plasma, only GHB-Gluc was detected, while both metabolites were clearly identified in urine, even in real human specimens. Stability was investigated under different temperature conditions for up to 4 weeks, and both phase II metabolites were found to be stable under refrigerated conditions. This method proved to be suitable for this purpose, and allowed for the first time the analysis and quantification of two different GHB metabolites from plasma and urine samples.

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Mehling, Lena-Maria UNSPECIFIED UNSPECIFIED UNSPECIFIED Piper, Thomas UNSPECIFIED orcid.org/0000-0002-7462-6693 UNSPECIFIED Dib, Josef UNSPECIFIED UNSPECIFIED UNSPECIFIED Pedersen, Daniel Sejer UNSPECIFIED orcid.org/0000-0003-3926-7047 UNSPECIFIED Madea, Burkhard UNSPECIFIED UNSPECIFIED UNSPECIFIED Hess, Cornelius UNSPECIFIED UNSPECIFIED UNSPECIFIED Thevis, Mario UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-247983
DOI:	10.1007/s11419-016-0339-4
Journal or Publication Title:	Forensic Toxicol.
Volume:	35
Number:	1
Page Range:	S. 77 - 86
Date:	2017
Publisher:	SPRINGER
Place of Publication:	NEW YORK
ISSN:	1860-8973
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language GAMMA-HYDROXYBUTYRIC ACID; HUMAN LIVER-MICROSOMES; MS/MS METHOD; IN-VITRO; METABOLITE; STABILITY Multiple languages Toxicology Multiple languages
Refereed:	Yes
URI:	http://kups.ub.uni-koeln.de/id/eprint/24798