Improved enantiomer resolution and quantification of free D-amino acids in serum and urine by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry

Wadhier, Magdalena C. and Almstetter, Martin F. and Nuernberger, Nadine and Gruber, Michael A. and Dettmer, Katja and Oefner, Peter J. (2011) Improved enantiomer resolution and quantification of free D-amino acids in serum and urine by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry. JOURNAL OF CHROMATOGRAPHY A, 1218 (28). pp. 4537-4544. ISSN 0021-9673,

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Abstract

The potential of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC x GC-TOFMS) in the quantitative analysis of amino acid enantiomers (AAEs) as their methyl chloroformate (MCF) derivatives in physiological fluids was investigated. Of the two column sets tested, the combination of an Rt-gamma DEXsa chiral column with a polar ZB-AAA column provided superior selectivity. Twenty AAEs were baseline resolved including L-Leu and D-Ile, which had failed separation by one-dimensional chiral GC-quadrupole-MS (GC-qMS). Lower limits of quantification (LLOQ) were in the range of 0.03-2 mu M. Reproducibility of the analysis of a serum specimen in octaplicate ranged from 1.3 to 16.6%. The GC x GC-TOFMS method was validated by analyzing AAEs in 48 urine and 43 serum specimens, respectively, and by comparing the results with data obtained by a previously validated GC-qMS method. Mean recoveries ranged from 78.4% for D-Leu to 116.4% for D-Pro in urine and 72.2% for L-Thr to 129.4% for L-Ile in serum. The method was applied to the comparison of AAE serum levels in patients suffering from liver cirrhosis to a control group. Significantly increased D-AA concentrations were found for the patient group, whereas L-AA levels were slightly decreased. (C) 2011 Elsevier B.V. All rights reserved.

Item Type: Article
Uncontrolled Keywords: GC-MS; MICROBIOLOGY; NUTRITION; OXIDASE; ORIGIN; PLASMA; FLUIDS; Enantioselective analysis; GC x GC-TOFMS; Methyl chloroformate; Metabolomics; Urine; Serum
Subjects: 600 Technology > 610 Medical sciences Medicine
Divisions: Medicine > Lehrstuhl für Anästhesiologie
Medicine > Institut für Funktionelle Genomik > Lehrstuhl für Funktionelle Genomik (Prof. Oefner)
Depositing User: Dr. Gernot Deinzer
Date Deposited: 05 Jun 2020 07:21
Last Modified: 05 Jun 2020 07:21
URI: https://pred.uni-regensburg.de/id/eprint/20537

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