Skip to main content

Determination of Andarine (S-4), a Selective Androgen Receptor Modulator, and Ibutamoren (MK-677), a Nonpeptide Growth Hormone Secretagogue, in Urine by Ultra-High Performance Liquid Chromatography with Tandem Mass-Spectrometric Detection

Abstract

A procedure for the determination of a selective androgen receptor modulator andarine (S-4) and a nonpeptide growth hormone secretagogue ibutamoren (MK-677) in urine has been developed including sample preparation by the “dilute-and-shoot” procedure, separation of analytes by ultra-high performance liquid chromatography in the gradient elution mode, and mass-spectrometric detection with heated electrospray ionization. The limits of detection are in the range of 0.5–2.5 ng/mL, the calibration curves are linear in the range of 2.5–250 ng/mL for andarine and 5–250 ng/mL for ibutamoren. The proposed procedure was used for the analysis of urine samples obtained from volunteers after a single administration of these drugs containing 15 mg of active substances.

This is a preview of subscription content, access via your institution.

References

  1. 1.

    Chen, J., Kim, J., and Dalton, J.T., Mol. Interventions, 2012, vol. 5, no. 3, p.173.

    Article  Google Scholar 

  2. 2.

    Aikawa, K., Miyawaki, T., Hitaka, T., Imai, Y.N., Hara, T., Miyazaki, J., Yamaoka, M., Kusaka, M., Kanzaki, N., Tasaka, A., Shiraishi, M., and Yamamoto, S., Bioorg. Med. Chem., 2015, vol. 23, no. 10, p. 2568.

    Article  CAS  PubMed  Google Scholar 

  3. 3.

    World Anti-Doping Agency, The World Anti-Doping Code, The 2008 Prohibited List, International Standard, 2008. www.wada-ama.org/sites/default/files/resources/files/WADA_Prohibited_List_2008_EN.pdf. Accessed May 7, 2017.

  4. 4.

    Gao, W., Kim, J., and Dalton, J.T., Pharm. Res., 2006, vol. 23, no. 8, p. 1641.

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  5. 5.

    Thevis, M., Kohler, M., Maurer, J., Schlorer, N., Kamber, M., and Schanzer, W., Rapid Commun. Mass. Spectrom., 2007, vol. 21, no. 21, p. 3477.

    Article  CAS  PubMed  Google Scholar 

  6. 6.

    Gao, W. and Dalton, J.T., Drug Discovery Today, 2007, vol. 12, nos. 5–6, p.241.

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  7. 7.

    Narayanan, R., Mohler, M.L., Bohl, C.E., Miller, D.D., and Dalton, J.T., Nucl. Recept. Signaling, 2008, vol. 6, p. e010.

    Article  Google Scholar 

  8. 8.

    Grata, E., Perrenoud, L., Saugy, M., and Baume, N., Forensic Sci. Int., 2011, vol. 213, nos. 1–3, p.104.

    Article  CAS  PubMed  Google Scholar 

  9. 9.

    Starcevic, B., Ahrens, B.D., and Butch, A.W., Drug Test. Anal., 2013, vol. 5, no. 5, p.377.

    Article  CAS  PubMed  Google Scholar 

  10. 10.

    Thevis, M., Thomas, A., Fußhöller, G., Beuck, S., Geyer, H., and Schänzer, W., Rapid Commun. Mass. Spectrom., 2010, vol. 24, no. 15, p. 2245.

    Article  CAS  PubMed  Google Scholar 

  11. 11.

    Patchett, A.A., Nargund, R.P., Tata, J.R., Chen,M.H., Barakat, K.J., Johnston, D.B., Cheng, K., Chan, W.W., Butler, B., and Hickey, G., Proc. Natl. Acad. Sci. U. S. A., 1995, vol. 92, no. 15, p. 7001.

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  12. 12.

    Smith, R.G., Endocr. Rev., 2005, vol. 26, no. 3, p.346.

    Article  CAS  PubMed  Google Scholar 

  13. 13.

    Sobolevsky, T., Krotov, G., Dikunets, M., Nikitina, M., Mochalova, E., and Rodchenkov, G., Drug Test. Anal., 2014, vol. 6, nos. 11–12, p. 1087.

    Article  CAS  PubMed  Google Scholar 

  14. 14.

    Sobolevsky, T., Prasolov, I., and Rodchenkov, G., Recent Adv. Doping Anal., 2013, p.182.

    Google Scholar 

  15. 15.

    Identification criteria for qualitative assays incorporating column chromatography and mass spectrometry, WADA Technical Document TD2015IDCR, 2015. www.wada-ama.org/sites/default/files/resources/files/td2015idcr_-_eng.pdf. Accessed May 7, 2017.

  16. 16.

    Cappiello, A., Famiglini, G., Palma, P., and Trufelli, H., J. Liq. Chromatogr., 2010, vol. 33, p. 1067.

    Article  CAS  Google Scholar 

  17. 17.

    Van Eeckhaut, A., Lanckmans, K., Sarre, S., Smolders, I., and Michotte, Y., J. Chromatogr. B: Anal. Technol. Biomed. Life Sci., 2009, vol. 877, no. 23, p. 2198.

    Article  CAS  Google Scholar 

  18. 18.

    Taylor, P.J., Clin. Biochem., 2005, vol. 38, no. 4, p.328.

    Article  CAS  PubMed  Google Scholar 

  19. 19.

    Deventer, K., Pozo, O.J., Verstraete, A.G., and Van Eenoo, P., TrAC, Trends. Anal. Chem., 2014, vol. 55, p.1.

    Article  CAS  Google Scholar 

  20. 20.

    FDA Guidance for Industry: Bioanalytical Method Validation, Rockville: US Department of Health and Human Services, Food and Drug Administration (FDA), 2013. https://doi.org/www.fda.gov/downloads/drugs/guidancecomplianceregulatoryinformation/guidances/ucm368107.pdf. Accessed May 7, 2017.

Download references

Author information

Affiliations

Authors

Corresponding author

Correspondence to E. V. Dmitrieva.

Additional information

Original Russian Text © E.V. Dmitrieva, A.Z. Temerdashev, A.A. Azaryan, E.M. Gashimova, 2018, published in Zhurnal Analiticheskoi Khimii, 2018, Vol. 73, No. 7, pp. 523–528.

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Dmitrieva, E.V., Temerdashev, A.Z., Azaryan, A.A. et al. Determination of Andarine (S-4), a Selective Androgen Receptor Modulator, and Ibutamoren (MK-677), a Nonpeptide Growth Hormone Secretagogue, in Urine by Ultra-High Performance Liquid Chromatography with Tandem Mass-Spectrometric Detection. J Anal Chem 73, 674–678 (2018). https://doi.org/10.1134/S1061934818070031

Download citation

Keywords

  • ultra-high performance liquid chromatography
  • tandem mass spectrometry
  • selective androgen receptor modulators
  • nonpeptide growth hormone secretagogue
  • andarine
  • ibutamoren
  • “dilute-and-shoot”
  • doping control