Validation of a headspace solid-phase microextraction–GC–MS/MS for the determination of ethyl glucuronide in hair according to forensic guidelines Ronald.

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Validation of a headspace solid-phase microextraction–GC–MS/MS for the determination of ethyl glucuronide in hair according to forensic guidelines Ronald Agius, Thomas Nadulski, Hans-Gerhard Kahl, Johannes Schräder, Bertin Dufaux, Michel Yegles, Fritz Pragst Forensic Science International Volume 196, Issue 1, Pages 3-9 (March 2010) DOI: 10.1016/j.forsciint.2009.07.023 Copyright © 2009 Elsevier Ireland Ltd Terms and Conditions

Fig. 1 Negative chemical ion mass spectra of (a) EtG and (b) EtG-d5 after derivatization with heptafluorobutyric acid anhydride in full scan mode. Forensic Science International 2010 196, 3-9DOI: (10.1016/j.forsciint.2009.07.023) Copyright © 2009 Elsevier Ireland Ltd Terms and Conditions

Fig. 2 EtG, EtG-PFPA and EtG-HFBA derivatives [26]. Forensic Science International 2010 196, 3-9DOI: (10.1016/j.forsciint.2009.07.023) Copyright © 2009 Elsevier Ireland Ltd Terms and Conditions

Fig. 3 Optimization of the SPME extraction time and the SPME extraction temperature for the determination of EtG in hair using HS-SPME and NCI-GC–MS; calculated by multivariate analysis (central composite design; CCD) [26]. (a) Temperature vs. extraction time 2D and (b) temperature vs. extraction time 3D. Forensic Science International 2010 196, 3-9DOI: (10.1016/j.forsciint.2009.07.023) Copyright © 2009 Elsevier Ireland Ltd Terms and Conditions

Fig. 4 (a) MRM chromatogram for a blank hair sample and (b) MRM chromatogram m/z 596→427 and m/z 596→288 for EtG in a spiked control at the cut-off concentration of 8pg/mg hair (peak to the right) with a signal to noise ratio of 447; MRM chromatogram m/z 601→432 and 601→288 for EtG-D5, used as an internal standard at 50pg/mg hair (peak to the left). Forensic Science International 2010 196, 3-9DOI: (10.1016/j.forsciint.2009.07.023) Copyright © 2009 Elsevier Ireland Ltd Terms and Conditions

Fig. 5 MRM chromatogram m/z 596→427 and m/z 596→288 for EtG in a real hair sample at the LLOQ level (2.8pg/mg hair) with a signal to noise ratio of 62. Forensic Science International 2010 196, 3-9DOI: (10.1016/j.forsciint.2009.07.023) Copyright © 2009 Elsevier Ireland Ltd Terms and Conditions

Fig. 6 Internal QC for EtG in hair for 20 separate days for spiked controls at (a) 8pg/mg, (b) 25pg/mg, (c) 40pg/mg and (d) 120pg/mg hair showing the calculated maximal permissible values using the rms deviations of measurement; Xo, target value; ULEL, upper laboratory error limits and LLEL, lower laboratory error limits. Forensic Science International 2010 196, 3-9DOI: (10.1016/j.forsciint.2009.07.023) Copyright © 2009 Elsevier Ireland Ltd Terms and Conditions

Fig. 7 Inter-laboratory comparisons between ethyl glucuronide concentration in hair samples measured in the Labor Krone and at the National Health Laboratory at the University of Luxembourg (Dr. Yegles). Forensic Science International 2010 196, 3-9DOI: (10.1016/j.forsciint.2009.07.023) Copyright © 2009 Elsevier Ireland Ltd Terms and Conditions

Fig. 8 The error profile based on the extended uncertainty of measurement U at 99% confidence intervals as a function of the calibration EtG levels in hair. Forensic Science International 2010 196, 3-9DOI: (10.1016/j.forsciint.2009.07.023) Copyright © 2009 Elsevier Ireland Ltd Terms and Conditions