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Analysis of Glycerol with Isolation of Endogenous Interferences using "Dilute and Shoot" Strategy and High-Resolution Mass Spectrometry in Human Urine for Antidoping Testing

  • Kim, Yongseok (Doping Control Center, Korea Institute of Science and Technology) ;
  • Min, Hophil (Doping Control Center, Korea Institute of Science and Technology) ;
  • Sung, Changmin (Doping Control Center, Korea Institute of Science and Technology) ;
  • Park, Ju-hyung (Doping Control Center, Korea Institute of Science and Technology) ;
  • Son, Junghyun (Doping Control Center, Korea Institute of Science and Technology) ;
  • Lee, Kang Mi (Doping Control Center, Korea Institute of Science and Technology) ;
  • Kim, Ho Jun (Doping Control Center, Korea Institute of Science and Technology) ;
  • Lee, Jaeick (Doping Control Center, Korea Institute of Science and Technology) ;
  • Kwon, Oh-Seung (Doping Control Center, Korea Institute of Science and Technology) ;
  • Kim, Ki Hun (Doping Control Center, Korea Institute of Science and Technology)
  • Received : 2016.11.30
  • Accepted : 2016.12.19
  • Published : 2016.12.30

Abstract

Glycerol was identified and isolated from endogenous interferences during analysis of human urine using high-resolution mass spectrometry (HRMS) for doping control. Urinary sample preparation was simple; the samples were diluted with an organic solvent and then analyzed using a liquid chromatography-mass spectrometry ("dilute and shoot" method). Although the interfering ion peaks were observed at the similar retention time of glycerol, the inference could be identified by isolation with HRMS and further investigation. Thus, creatinine was identified as the endogenous interference for glycerol analysis and it also caused ion suppression resulting in the decrease of glycerol signal. This study reports the first identification and efficient isolation of endogenous interferences in human urine for "dilute and shoot" method. The information about ion suppression could be novel to prevent overestimation or a false result for antidoping analysis.

Keywords

References

  1. WADA. The 2016 prohibited list international standard, https://www.wada-ama.org/en/international-standards. 2016.
  2. Polyviou, T. P.; Easton, C.; Beis, L.; Malkova, D.; Takas, P.; Hambly, C.; Speakman, J. R.; Koehler, K.; Pitsiladis, Y. P. Nutr. 2012, 4, 1171.
  3. Nash, T. Biochem. J. 1953, 55, 416. https://doi.org/10.1042/bj0550416
  4. Thevis, M.; Guddat, S.; Flenker, U.; Schanzer, W. Eur. J. Mass Spectrom. 2008, 14, 117. https://doi.org/10.1255/ejms.919
  5. Dong, Y.; Yan, K.; Ma, Y.; Yang, Z.; Zhao, J.; Ding, J. J. Chromatogr. B 2016, 1022, 153. https://doi.org/10.1016/j.jchromb.2016.04.023
  6. Dong, Y.; Ma, Y.; Yan, K.; Shen, L.; Wang, X.; Xu, Y.; He, G.; Wu, Y.; Lu, J.; Yang, Z.; Feng, F. J. Chromatogr. B 2014, 957, 30. https://doi.org/10.1016/j.jchromb.2014.02.054
  7. Jeong, E. S.; Kim, S. H.; Cha, E. J.; Lee, K. M.; Kim, H. J.; Lee, S. W.; Kwon, O. S.; Lee, J. Rapid Commun. Mass Spectrom. 2015, 29, 367. https://doi.org/10.1002/rcm.7113
  8. Gorgens, C.; Guddat, S.; Orlovius, A. K.; Sigmund, G.; Thomas, A.; Thevis, M.; Schanzer, W. Anal. Bioanal. Chem. 2015, 407, 5365. https://doi.org/10.1007/s00216-015-8699-x
  9. Jimenez Giron, A.; Deventer, K.; Roels, K.; Van Eenoo, P. Anal. Chim. Acta 2012, 721, 137. https://doi.org/10.1016/j.aca.2012.02.002
  10. Guddat, S.; Solymos, E.; Orlovius, A.; Thomas, A.; Sigmund, G.; Geyer, H.; Thevis, M.; Schanzer, W. Drug Test. Anal. 2011, 3, 836. https://doi.org/10.1002/dta.372
  11. Fitzgerald, R. L.; Griffin, T. L.; Yun, Y. M.; Godfrey, R. A.; West, R.; Pesce, A. J.; Herold, D. A. J. Anal. Toxicol. 2012, 36, 106. https://doi.org/10.1093/jat/bkr024
  12. Beck, O.; Ericsson, M. Bioanalysis 2014, 6, 2229. https://doi.org/10.4155/bio.14.192
  13. Annesley, T. M. Clin. Chem. 2003, 49, 1041. https://doi.org/10.1373/49.7.1041
  14. Schlittenbauer, L.; Seiwert, B.; Reemtsma, T. Rapid Commun. Mass Spectrom. 2016, 1560.