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Development and validation of a fast gas chromatography combustion isotope ratio mass spectrometry method for the detection of epiandrosterone sulfate in urine

Laurie De Wilde (UGent) , Pieter Van Renterghem (UGent) , Peter Van Eenoo (UGent) and Michaël Polet (UGent)
(2020) DRUG TESTING AND ANALYSIS. 12(8). p.1006-1018
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Abstract
In doping control, to confirm the exogenous origin of exogenously administered anabolic androgenic steroids (AAS), a gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) analysis is performed. Recently published work suggests that epiandrosterone sulfate (EpiAS) is a promising IRMS target compound for the detection of AAS, capable of prolonging the detection window. However, EpiAS is only excreted in urine in its sulfoconjugated form, while all other IRMS target compounds are excreted glucuronidated, meaning that EpiAS cannot be incorporated in the existing IRMS methods. A separate extensive sample preparation needs to be performed on this compound with a different hydrolysis and extraction procedure and a different liquid chromatography (LC) clean-up. The current work presents a new, fast, and easy to implement EpiAS IRMS method. The approach was based on the direct GC analysis of non-hydrolyzed EpiAS, making the solid phase extraction, hydrolysis, and acetylation step redundant. Sample preparation consisted of a simple liquid-liquid extraction, followed by LC fraction collection. A population study was performed to check compliance with the criteria drafted by the World Anti-Doping Agency (WADA). To verify the applicability of the developed approach, the method was applied to the samples of four administration studies (i.e. dehydroepiandrosterone (DHEA), testosterone gel (T gel), androstenedione (ADION), and intramuscular testosterone undecanoate. In contrast to previously published data, the strength of EpiAS as the target compound and the prolongation of the detection window in comparison with the conventional IRMS target compounds was less pronounced.
Keywords
Analytical Chemistry, Spectroscopy, Pharmaceutical Science, Environmental Chemistry, doping, epiandrosterone sulfate, isotope ratio mass spectrometry, steroids, urine, C-13/C-12 RATIOS, IDENTIFICATION, TESTOSTERONE, METABOLISM, STEROIDS, HORSE, 1-DEHYDROTESTOSTERONE

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Citation

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MLA
De Wilde, Laurie, et al. “Development and Validation of a Fast Gas Chromatography Combustion Isotope Ratio Mass Spectrometry Method for the Detection of Epiandrosterone Sulfate in Urine.” DRUG TESTING AND ANALYSIS, vol. 12, no. 8, 2020, pp. 1006–18, doi:10.1002/dta.2801.
APA
De Wilde, L., Van Renterghem, P., Van Eenoo, P., & Polet, M. (2020). Development and validation of a fast gas chromatography combustion isotope ratio mass spectrometry method for the detection of epiandrosterone sulfate in urine. DRUG TESTING AND ANALYSIS, 12(8), 1006–1018. https://doi.org/10.1002/dta.2801
Chicago author-date
De Wilde, Laurie, Pieter Van Renterghem, Peter Van Eenoo, and Michaël Polet. 2020. “Development and Validation of a Fast Gas Chromatography Combustion Isotope Ratio Mass Spectrometry Method for the Detection of Epiandrosterone Sulfate in Urine.” DRUG TESTING AND ANALYSIS 12 (8): 1006–18. https://doi.org/10.1002/dta.2801.
Chicago author-date (all authors)
De Wilde, Laurie, Pieter Van Renterghem, Peter Van Eenoo, and Michaël Polet. 2020. “Development and Validation of a Fast Gas Chromatography Combustion Isotope Ratio Mass Spectrometry Method for the Detection of Epiandrosterone Sulfate in Urine.” DRUG TESTING AND ANALYSIS 12 (8): 1006–1018. doi:10.1002/dta.2801.
Vancouver
1.
De Wilde L, Van Renterghem P, Van Eenoo P, Polet M. Development and validation of a fast gas chromatography combustion isotope ratio mass spectrometry method for the detection of epiandrosterone sulfate in urine. DRUG TESTING AND ANALYSIS. 2020;12(8):1006–18.
IEEE
[1]
L. De Wilde, P. Van Renterghem, P. Van Eenoo, and M. Polet, “Development and validation of a fast gas chromatography combustion isotope ratio mass spectrometry method for the detection of epiandrosterone sulfate in urine,” DRUG TESTING AND ANALYSIS, vol. 12, no. 8, pp. 1006–1018, 2020.
@article{8660256,
  abstract     = {{In doping control, to confirm the exogenous origin of exogenously administered anabolic androgenic steroids (AAS), a gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) analysis is performed. Recently published work suggests that epiandrosterone sulfate (EpiAS) is a promising IRMS target compound for the detection of AAS, capable of prolonging the detection window. However, EpiAS is only excreted in urine in its sulfoconjugated form, while all other IRMS target compounds are excreted glucuronidated, meaning that EpiAS cannot be incorporated in the existing IRMS methods. A separate extensive sample preparation needs to be performed on this compound with a different hydrolysis and extraction procedure and a different liquid chromatography (LC) clean-up.

The current work presents a new, fast, and easy to implement EpiAS IRMS method. The approach was based on the direct GC analysis of non-hydrolyzed EpiAS, making the solid phase extraction, hydrolysis, and acetylation step redundant. Sample preparation consisted of a simple liquid-liquid extraction, followed by LC fraction collection. A population study was performed to check compliance with the criteria drafted by the World Anti-Doping Agency (WADA). To verify the applicability of the developed approach, the method was applied to the samples of four administration studies (i.e. dehydroepiandrosterone (DHEA), testosterone gel (T gel), androstenedione (ADION), and intramuscular testosterone undecanoate. In contrast to previously published data, the strength of EpiAS as the target compound and the prolongation of the detection window in comparison with the conventional IRMS target compounds was less pronounced.}},
  author       = {{De Wilde, Laurie and Van Renterghem, Pieter and Van Eenoo, Peter and Polet, Michaël}},
  issn         = {{1942-7603}},
  journal      = {{DRUG TESTING AND ANALYSIS}},
  keywords     = {{Analytical Chemistry,Spectroscopy,Pharmaceutical Science,Environmental Chemistry,doping,epiandrosterone sulfate,isotope ratio mass spectrometry,steroids,urine,C-13/C-12 RATIOS,IDENTIFICATION,TESTOSTERONE,METABOLISM,STEROIDS,HORSE,1-DEHYDROTESTOSTERONE}},
  language     = {{eng}},
  number       = {{8}},
  pages        = {{1006--1018}},
  title        = {{Development and validation of a fast gas chromatography combustion isotope ratio mass spectrometry method for the detection of epiandrosterone sulfate in urine}},
  url          = {{http://dx.doi.org/10.1002/dta.2801}},
  volume       = {{12}},
  year         = {{2020}},
}

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