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A uniform sample preparation procedure for gas chromatography combustion isotope ratio mass spectrometry for all human doping control relevant anabolic steroids using online 2/3-dimensional liquid chromatography fraction collection

Lenka Honesová (UGent) , Peter Van Eenoo (UGent) and Michaël Polet (UGent)
(2021) Proceedings of the Manfred Donike Workshop : 39th Cologne Workshop on Dope Analysis, 22nd to 26th March 2021. In Recent Advances in Doping Analysis 29. p.213-214
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Abstract
Androgenic anabolic steroids are the most misused substances in sports because of their performance-enhancing effects. Often synthetic analogues of endogenously present steroids are administered. To determine their endogenous or exogenous origin, Gas Chromatography Combustion Isotope Ratio Mass Spectrometry (GC-C-IRMS) is used in the field of doping control. Compounds subjected to IRMS analysis must be interference-free, with liquid chromatography fraction collection (HPLC-FC) being the crucial clean-up step. This clean-up is challenging, particularly for compounds present at low concentrations in samples with pronounced matrix effects. Currently, the available methods only deal with a selection of the compounds mentioned above. Some of these compounds (e.g., 19-NA, B, BM, 6aOHADION) are present in very low concentrations, requiring an extensive sample clean-up, making it challenging to develop a universal clean-up procedure. Many of these methods require different and multiple offline HPLC-FC set-ups, which can be labour-intensive and time-consuming. That is problematic during, e.g., large sports events, where reporting time is limited to 72 hours. Therefore, we developed a uniform online 2D/3D HPLC-FC method (set-up described in Figure 1), capable of purifying all relevant target compounds in a single run, leading to the fastest clean-up procedure so far (i.e., 31 min for T and its main metabolites; 46 min for 19-NA, F and 6aOHADION; 48 min for B and BM). A satisfactory clean-up was demonstrated by the excellent accuracy obtained during the analysis of certified samples and EQAS samples. This method was fully compliant with WADA requirements with LOQs of 2 ng mL for 6aOHADION-Ac, B-Ac, BM-Ac and 19-NA-Ac and of 10 ng mL for T-Ac and its metabolites and F-Ac. This work demonstrates the possibilities of multi-dimensional HPLC as an automated multi-target sample preparation methodology and how finding an optimal set-up allows pushing analytical instruments to their maximal capabilities.

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MLA
Honesová, Lenka, et al. “A Uniform Sample Preparation Procedure for Gas Chromatography Combustion Isotope Ratio Mass Spectrometry for All Human Doping Control Relevant Anabolic Steroids Using Online 2/3-Dimensional Liquid Chromatography Fraction Collection.” Proceedings of the Manfred Donike Workshop : 39th Cologne Workshop on Dope Analysis, 22nd to 26th March 2021, edited by Mario Thevis et al., vol. 29, Sportverlag Strauß, 2021, pp. 213–14.
APA
Honesová, L., Van Eenoo, P., & Polet, M. (2021). A uniform sample preparation procedure for gas chromatography combustion isotope ratio mass spectrometry for all human doping control relevant anabolic steroids using online 2/3-dimensional liquid chromatography fraction collection. In M. Thevis, H. Geyer, & U. Mareck (Eds.), Proceedings of the Manfred Donike Workshop : 39th Cologne Workshop on Dope Analysis, 22nd to 26th March 2021 (Vol. 29, pp. 213–214). Cologne: Sportverlag Strauß.
Chicago author-date
Honesová, Lenka, Peter Van Eenoo, and Michaël Polet. 2021. “A Uniform Sample Preparation Procedure for Gas Chromatography Combustion Isotope Ratio Mass Spectrometry for All Human Doping Control Relevant Anabolic Steroids Using Online 2/3-Dimensional Liquid Chromatography Fraction Collection.” In Proceedings of the Manfred Donike Workshop : 39th Cologne Workshop on Dope Analysis, 22nd to 26th March 2021, edited by Mario Thevis, Hans Geyer, and Ute Mareck, 29:213–14. Cologne: Sportverlag Strauß.
Chicago author-date (all authors)
Honesová, Lenka, Peter Van Eenoo, and Michaël Polet. 2021. “A Uniform Sample Preparation Procedure for Gas Chromatography Combustion Isotope Ratio Mass Spectrometry for All Human Doping Control Relevant Anabolic Steroids Using Online 2/3-Dimensional Liquid Chromatography Fraction Collection.” In Proceedings of the Manfred Donike Workshop : 39th Cologne Workshop on Dope Analysis, 22nd to 26th March 2021, ed by. Mario Thevis, Hans Geyer, and Ute Mareck, 29:213–214. Cologne: Sportverlag Strauß.
Vancouver
1.
Honesová L, Van Eenoo P, Polet M. A uniform sample preparation procedure for gas chromatography combustion isotope ratio mass spectrometry for all human doping control relevant anabolic steroids using online 2/3-dimensional liquid chromatography fraction collection. In: Thevis M, Geyer H, Mareck U, editors. Proceedings of the Manfred Donike Workshop : 39th Cologne Workshop on Dope Analysis, 22nd to 26th March 2021. Cologne: Sportverlag Strauß; 2021. p. 213–4.
IEEE
[1]
L. Honesová, P. Van Eenoo, and M. Polet, “A uniform sample preparation procedure for gas chromatography combustion isotope ratio mass spectrometry for all human doping control relevant anabolic steroids using online 2/3-dimensional liquid chromatography fraction collection,” in Proceedings of the Manfred Donike Workshop : 39th Cologne Workshop on Dope Analysis, 22nd to 26th March 2021, Cologne, Germany (Online), 2021, vol. 29, pp. 213–214.
@inproceedings{01J3Z3668XTJ2XPQHRSGS3PT2Z,
  abstract     = {{Androgenic anabolic steroids are the most misused substances in sports because of their performance-enhancing
effects. Often synthetic analogues of endogenously present steroids are administered. To determine their endogenous or exogenous origin, Gas Chromatography Combustion Isotope Ratio Mass Spectrometry (GC-C-IRMS) is used in the field of doping control. Compounds subjected to IRMS analysis must be interference-free, with liquid chromatography fraction collection (HPLC-FC) being the crucial clean-up step. This clean-up is challenging, particularly for compounds present at low concentrations in samples with pronounced matrix effects. Currently, the available methods only deal with a selection of the compounds mentioned above. Some of these compounds (e.g., 19-NA, B, BM, 6aOHADION) are present in very low concentrations, requiring an extensive sample clean-up, making it challenging to develop a universal clean-up procedure. Many of these methods require different and multiple offline HPLC-FC set-ups, which can be labour-intensive and time-consuming. That is problematic during, e.g., large sports events, where reporting time is limited to 72 hours.

Therefore, we developed a uniform online 2D/3D HPLC-FC method (set-up described in Figure 1), capable
of purifying all relevant target compounds in a single run, leading to the fastest clean-up procedure so far
(i.e., 31 min for T and its main metabolites; 46 min for 19-NA, F and 6aOHADION; 48 min for B and BM). A
satisfactory clean-up was demonstrated by the excellent accuracy obtained during the analysis of
certified samples and EQAS samples. This method was fully compliant with WADA requirements with
LOQs of 2 ng mL for 6aOHADION-Ac, B-Ac, BM-Ac and 19-NA-Ac and of 10 ng mL for T-Ac and its
metabolites and F-Ac.

This work demonstrates the possibilities of multi-dimensional HPLC as an automated multi-target sample
preparation methodology and how finding an optimal set-up allows pushing analytical instruments to
their maximal capabilities.}},
  author       = {{Honesová, Lenka and Van Eenoo, Peter and Polet, Michaël}},
  booktitle    = {{Proceedings of the Manfred Donike Workshop : 39th Cologne Workshop on Dope Analysis, 22nd to 26th March 2021}},
  editor       = {{Thevis, Mario and Geyer, Hans and Mareck, Ute}},
  isbn         = {{9783868840476}},
  language     = {{eng}},
  location     = {{Cologne, Germany (Online)}},
  pages        = {{213--214}},
  publisher    = {{Sportverlag Strauß}},
  title        = {{A uniform sample preparation procedure for gas chromatography combustion isotope ratio mass spectrometry for all human doping control relevant anabolic steroids using online 2/3-dimensional liquid chromatography fraction collection}},
  url          = {{https://www.dshs-koeln.de/fileadmin/redaktion/Institute/Biochemie/PDF/Proceedings/Proceedings_29/Recent_Advances_in_Doping_Analysis_29_2021.pdf}},
  volume       = {{29}},
  year         = {{2021}},
}