Application of chromatography and mass-spectrometry for the complex toxicological expertices

  • Azamat Z. Temerdashev Kuban State University, Krasnodar
  • Elina M. Gashimova Kuban State University, Krasnodar
Keywords: ephedrine, ethanol, steroids, testosterone, UHPLC-MS/MS, GC-MS, .

Abstract

In recent years, the promotion of sports and healthy lifestyles has been conducted as part of governmental
programs all over the world. The number of people involved in sports is steadily growing and as a
consequence a shadow market of performance-enhancing drugs and supplements also increases. Such drugs
often contain compounds banned by the World Anti-Doping Agency (WADA).
A wide range of compounds is included in the Prohibited list: stimulants, anabolic agents, different
non-approved substances, etc., however, they are still available on the free market and can be found even in
sports nutrition. The temptation to experiment with these supplements is huge for lots of athletes. Moreover,
manufacturers claim the necessity of food supplements in order to perform better and to be competitive. As a
result, even anabolic agents can be found in sports nutrition. For the class of “fatburners” the presence of
prohibited ephedrine, synephrine and methylsynephrine is common. In some cases, supplements contained
banned substances not indicated on the label.
An unexpected death case is presented in this article. It might have happened because of an unacceptable
combination of alcohol, ephedrine, anabolic agents and heavy training. The results of post-mortem
expertise using ultra-high performance liquid chromatography-tandem mass-spectrometry (UHPLC-MS/MS),
gas chromatography-mass spectrometry (GC-MS) and headspace gas chromatography combined with flame
ionization detection (HS-GC-FID) are presented. The presence of exogenous testosterone in urine was suspected
due to abnormally high testosterone/epitestosterone ratio (9:1) along with the total testosterone concentration
of 130 ng/mL. Ephedrine was found as a component of a fatburner and its concentration in urine
was 12 μg/mL. The presence of ethanol in blood was confirmed by HS-GC-FID and its concentration was
0.3 mg/L. LODs for ephedrine and testosterone evaluated by UHPLC-MS/MS determination in urine were
0.005 μg/mL and 0.05 ng/mL, respectively. LOQ for HS-GC-FID determination of ethanol in blood was 0.1
mg/L.

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Author Biographies

Azamat Z. Temerdashev, Kuban State University, Krasnodar

assistant professor, Ph.D., analytical chemistry department, Kuban State University, Krasnodar, e-mail: TemerdashevAZ@gmail.com

Elina M. Gashimova, Kuban State University, Krasnodar

Ph.D. student, analytical chemistry department, Kuban State University, Krasnodar, e-mail: elina.gashimova@yandex.ru

References

1. World Anti-Doping Agency. The World Anti-Doping Code. The 2019 Prohibited List. International Standard. Available at:https://www.wadaama.org/sites/default/files/wada_2019_english_prohibited_list.pdf (accessed 22 August 2019).
2. Thevis M., Kuuranne T., Geyer H., Drug Test. Anal., 2018, Vol. 10, pp. 9-27. doi:10.1002/dta.2336
3. De Cock K.J.S., Delbeke F.T., Van Eenoo P., Desmet N. et al., J. Pharm. Biomed. Anal., 2001, Vol. 25, pp. 843-852. doi:10.1016/S0731-7085(01)00396-X
4. de Hon O., Coumans B., British J. Sports Med., 2007, Vol. 41, pp. 800-805. doi:10.1136/bjsm.2007.037226
5. Furjan Mandic G., Peric M., Krzelj L., Stankovic S. et al., J. Sports Sci. Med., 2013, Vol. 12, pp. 753-760.
6. Morente-Sánchez J., Zabala M., Sports Med., 2013, Vol. 43, pp. 395-411. doi:10.1007/s40279-013-0037-x7. Temerdashev A.Z., Azaryan A.A., Labutin A.V., Dikunets M.A. et al., J. Anal. Chem., 2017, Vol. 72, pp. 1184-1192. doi:10.1134/s1061934817110090
8. Asatryan B., Vital C., Kellerhals C., Medeiros- Domingo A., Grani C., Trashsel L.D., Schied C.M., Saguner A.M., Eser P., Herzig D., Bolliger S., Michaud K., Willhelm M., PLOS ONE, 2017, Vol. 12, pp. e0174434. doi:10.1371/journal.pone.0174434
9. Halabchi F., Seif-Barghi T., Mazaheri R., Asian J. Sports Med., 2011, Vol. 2, pp. 1-15.
10. Tiscione N.B., Alford I., Yeatman D.T., Shan X., J. Anal. Tox., 2011, Vol. 35, pp. 501-511. doi:10.1093/anatox/35.7.501
11. Kristoffersen L., Stormyhr L.-E., Smith-Kielland A., Forensic Sci. Int., 2006, Vol. 161, pp. 151-157. doi:10.1016/j.forsciint.2006.03.034
12. Shan X., Tiscione N.B., Alford I., Yeatman D.T., Forensic Sci. Int., 2011, Vol. 211, pp. 47-50. doi: 10.1016/j.forsciint.2011.04.012.
13. Wasfi I.A., Al-Awadhi A.H., Al-Hatali Z.N., Al-Rayami F.J. et al., J. Chromatogr. B, 2004, Vol. 799, pp. 331-336. doi:10.1016/j.jchromb.2003.11.003
14. WADA Technical Document – TD2016EAAS. Endogenous Anabolic Androgenic Steroids Measurement and Reporting.
Available at: https://www.wadaama.org/sites/default/files/resources/files/wadatd2016eaas-eaas-measurement-and-reportingen.pdf (accessed 19 August 2019)
Published
2019-10-30
How to Cite
Temerdashev, A. Z., & Gashimova, E. M. (2019). Application of chromatography and mass-spectrometry for the complex toxicological expertices. Sorbtsionnye I Khromatograficheskie Protsessy, 19(5), 542-549. https://doi.org/10.17308/sorpchrom.2019.19/1168