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Study of Dolutegravir Degradation and Spectroscopic Identification of Products by LCMS, 1H and 13C NMR Techniques

  • T. N. V. Ganesh KumarEmail author
  • S. Vidyadhara
  • Niteen A. Narkhede
  • N. Soundarya
Article

Stability study for dolutegravir bulk drug was performed and the degradation products formed were identified by chromatography (HPLC, LCMS) and spectroscopy (ESI-MS, FTIR, 1H and 13C NMR) techniques. Degradation of the drug in acidic and peroxide environment yielded one common major degradant f ((2,4-difluorophenyl) methanamine) with a mass peak at m/z = 182.44. In addition to this, five more minor degradation products (a, b, c, d and e) were formed. The structure interpretation showed that the drug degraded to its synthetic precursor and no extra structures were formed. Hence, it was suggested that drug dolutegravir should be kept away from acidic and oxygen rich conditions.

Keywords

dolutegravir degradation spectroscopy LCMS, NMR 

Notes

Conflict of Interest

The authors declare no conflict of interest.

References

  1. 1.
    British National Formulary: BNF 69 (69th Edition), British Medical Association (2015), 429.ISBN 9780857111562.Google Scholar
  2. 2.
    S. Kanters, M. Vitoria, M. Doherty, et al., Lancet HIV, 3, 510–520 (2016).CrossRefGoogle Scholar
  3. 3.
    N. Mulligan, B. Best, E. Capparelli, et al., in: Conference on Retroviruses and Opportunistic Infections (2016, Boston, MA, USA), Abstract 438.Google Scholar
  4. 4.
    G. B. Bhavar, S. S. Pekamwar, K. B. Aher, et al., Sci. Pharm., 84(2), 305 – 320 (2016).CrossRefGoogle Scholar
  5. 5.
    G. B. Bhavar, K. B. Aher, R. S. Thorat, et al., Malay. J. Anal. Sci., 19(6), 1156 – 1163 (2015).Google Scholar
  6. 6.
    N. M. Rao and D. G. Sankar, Future J. Pharm. Sci., 1(2), 73 – 77 (2015).CrossRefGoogle Scholar
  7. 7.
    X. Wang, S. D. Penchala, A. Amara, et al., Ther. Drug Monitor., 38(3), 327 – 31 (2016).CrossRefGoogle Scholar
  8. 8.
    ICH Q2 (R1), Validation of Analytical Procedures: Text and Methodology. International Conference on Harmonization, IFPMA, World Health Organization: Geneva (2009).Google Scholar
  9. 9.
    M. Nenad, Lovro Selic, and C. Anja, Patent WO2016113372A1 (2016).Google Scholar

Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2019

Authors and Affiliations

  • T. N. V. Ganesh Kumar
    • 1
    Email author
  • S. Vidyadhara
    • 1
  • Niteen A. Narkhede
    • 2
  • N. Soundarya
    • 1
  1. 1.Chebrolu Hanumaiah Institute of Pharmaceutical SciencesGunturIndia
  2. 2.Indian Institute of Integrative MedicineMumbaiIndia

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