Application of comprehensive two-dimensional gas chromatography to sterols analysis

Mitrevski, B, Brenna, T, Zhang, Y and Marriott, P 2008, 'Application of comprehensive two-dimensional gas chromatography to sterols analysis', Journal of Chromatography A, vol. 1214, no. 1-2, pp. 134-142.


Document type: Journal Article
Collection: Journal Articles

Title Application of comprehensive two-dimensional gas chromatography to sterols analysis
Author(s) Mitrevski, B
Brenna, T
Zhang, Y
Marriott, P
Year 2008
Journal name Journal of Chromatography A
Volume number 1214
Issue number 1-2
Start page 134
End page 142
Total pages 8
Publisher Elsevier
Abstract The applicability of comprehensive two-dimensional gas chromatography (GC×GC) for sterol analysis was investigated by separation and identification of endogenous sterols in standards, and spiked in human urine. The modulation temperature was optimized to achieve the best separation and signal enhancement. The separation pattern of trimethylsilyl (TMS) derivatives of sterols was compared on two complementary column sets. Whilst the BPX5/BPX50 column set offers better overall separation, BPX50/BPX5 provides better peak shape and sensitivity. Comparison of the identification power of GC×GC--TOFMS against both the NIST05 MS library and a laboratory created (in-house) TOFMS library was carried out on a free sterols extract of urine, derivatised and spiked at the World Anti-Doping Agency (WADA) limit of 2 ng mL-1. The average match quality for 19 analysed sterols on the BPX50/BPX5 column set was 950/1000 when searched against the in-house library; only four were identified against the NIST05 library, at a match threshold of 800. The match quality of GC×GC--TOFMS spectra was superior to that for analysis using 1D GC--TOFMS for sterols spiked in urine at 10 ng mL-1. An r2 > 0.997 was obtained for the concentration range between 0.25 ng mL-1 and 10 ng mL-1 for three selected sterols. The lowest limit of detection (LOD) was obtained for estrone (0.1 ng mL-1) and the highest LOD was for 5a-androstan-3a,11ß-diol-17-one, epitestosterone and cholesteryl butyrate (1 ng mL-1), using a match threshold of at least 800 and signal-to-noise ratio of at least 10. TOFMS coupled to GC×GC enabled satisfactory identification of sterols in urine at their LOD. A minimum acceptable match (MAM) criterion for urinary sterols using 2D retention times and TOF mass spectra is introduced. This study shows that GC×GC--TOFMS yields high specificity for steroids derived from urine, with detection limits appropriate for use in doping control.
Subject Separation Science
DOI - identifier 10.1016/j.chroma.2008.10.045
Copyright notice Copyright © 2008 Elsevier B.V. All rights reserved.
ISSN 0021-9673
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