Journal of Radioanalytical and Nuclear Chemistry

, Volume 295, Issue 3, pp 2163–2170 | Cite as

The identity confirmation of 99gTc-DMSA complexes by using NMR and HPLC–MS/MS methods

  • R. Staník
  • I. Benkovský
  • J. Světlík
  • J. Galba
  • N. Prónayová
  • J. Karlovská


The analyses of 99gTc-DMSA complexes prepared under alkali and acidic reactions were reported. Modern analytical, separation and spectral methods such as NMR (1H-NMR, 13C-NMR, APT, COSY and HSQC) and Q-TOF HPLC–MS/MS system with ESI were employed to determine the identity and characterization of the products. The structure of 99gTc(V)DMSA was clearly confirmed and its fragmentation path in negative and positive ionisation mode was suggested. The effect of ascorbic acid and new alternative labelling with the use of NH 4 99g TcOCl4 was examined. Surprisingly, 99gTc(III)DMSA complex was not formed under acidic reaction conditions. 99gTc(V)DMSA complex was the main reaction product under both experimental conditions. This result suggests the key role of 99g/99mTc concentration during the process of radiopharmaceuticals preparation.





The authors wish to thank the Grant Agency of Slovak Republic (Grant No. 1/0429/11; Grant No. 1/0664/12) and the Comenius University (Grant No. UK/86/2012) for their financial support. The authors would like to thank Dr. Jean-Luc Vanderheyden and Dr. Silvia Jurisson for their valuable advices and discussion.

Supplementary material

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  1. 1.
    Camacho V, Estroch M, Fraga G et al (2004) Eur J Nucl Med Mol Imaging 31:862CrossRefGoogle Scholar
  2. 2.
    Grattan-Smith JD, Little SB, Jones RA (2008) Pediatr Radiol 38:S83CrossRefGoogle Scholar
  3. 3.
    Gilani KA, Esfeh JM, Gholamrezanezhad A et al (2010) Int Urol Nephrol 42:1041CrossRefGoogle Scholar
  4. 4.
    Patel MC, Ramanathan P, Ramamoorthy N et al (1988) Eur J Nucl Med 13:507CrossRefGoogle Scholar
  5. 5.
    Hirano T, Otake H, Yoshida I et al (1995) J Nucl Med 36:202Google Scholar
  6. 6.
    Adams S, Baum RP, Hertel A et al (1998) Eur J Nucl Med 25:1277CrossRefGoogle Scholar
  7. 7.
    Papantoniou V, Valsamaki P, Sotiropoulos E et al (2011) Mol Imaging 10:370Google Scholar
  8. 8.
    Ergun EL, Kara PO, Gedik GK et al (2007) Ann Nucl Med 21:275CrossRefGoogle Scholar
  9. 9.
    Kiratli PO, Kiratli H, Ercan MT (1998) Ann Nucl Med 21:157CrossRefGoogle Scholar
  10. 10.
    Horiuchi-Suzuki K, Konno A, Ueda M et al (2004) Eur J Nucl Med Mol Imaging 31:388CrossRefGoogle Scholar
  11. 11.
    Trapali X, Yissimopoulos A, Baziotis N et al (1992) J Nucl Med 33:708Google Scholar
  12. 12.
    Lam ASK, Kettle AG, O`Doherty MJ et al (1997) Nucl Med Commun 18:907CrossRefGoogle Scholar
  13. 13.
    Moretti JL, Rapin JR, Saccavini JC et al (1984) Int J Nucl Med Biol 11:270CrossRefGoogle Scholar
  14. 14.
    Blower PJ, Singh J, Clarke SEM (1991) J Nucl Med 32:845Google Scholar
  15. 15.
    Zolle I (2007) Technetium-99 m pharmaceuticals. Springer, Berlin. ISBN 10 3-540-33989-2Google Scholar
  16. 16.
    Hill DM, Barnes RK, Wong HKY et al (2000) Appl Radiat Isot 53:415CrossRefGoogle Scholar
  17. 17.
    Jovanović V, Maksin T, Konstantinovska D et al (1980) J Radioanal Chem 59:239CrossRefGoogle Scholar
  18. 18.
    Archimandritis SC, Belkas EP (1986) J Radioanal Nucl Chem 100:381CrossRefGoogle Scholar
  19. 19.
    Vanderghinste D, Van Eeckhoudt M, Terwinghe C et al (2003) J Pharma Biol Anal 32:679CrossRefGoogle Scholar
  20. 20.
    Vanbilloen HP, Cleynhens BJ, de Groot TJ et al (2003) J Pharma Biol Anal 32:663CrossRefGoogle Scholar
  21. 21.
    Verduyckt T, Kieffer D, Huyghe D et al (2003) J Pharma Biol Anal 32:669CrossRefGoogle Scholar
  22. 22.
    Rattat D, Cleynhens B, Bormans G et al (2005) Bioorg Med Chem Lett 15:4192CrossRefGoogle Scholar
  23. 23.
    King RC, Surfraz MBU, Biagini SCG et al (2007) Dalton Trans 43:4998CrossRefGoogle Scholar
  24. 24.
    Tarasov VP, Muravlev YB, German KE et al (2001) Phys Chem 377:71Google Scholar
  25. 25.
    O’Connel LA, Pearlstein RM, Davison A et al (1989) Inorg Chim Acta 161:39CrossRefGoogle Scholar
  26. 26.
    Helm L (2008) Coord Chem Rev 252:2346CrossRefGoogle Scholar
  27. 27.
    Tisato F, Parchia M, Bolzati C et al (2006) Coord Chem Rev 250:2034CrossRefGoogle Scholar
  28. 28.
    Davison A, Jones AG (1982) Int J Appl Radiat Isot 33:875CrossRefGoogle Scholar
  29. 29.
    Westera G, Gadze A, Horst W (1984) Int J Appl Radiat Isot 36:311CrossRefGoogle Scholar
  30. 30.
    Staník R, Světlík J, Karlovská J et al (2011) J Radioanal Nucl Chem 289:909CrossRefGoogle Scholar
  31. 31.
    Spies H, Scheller D (1986) Inorg Chim Acta 116:1CrossRefGoogle Scholar
  32. 32.
    Jameson CJ, Mason J (1987) In: Mason J (ed) Multinuclear NMR. Plenum Press, New York, ISBN 0-306-42153-4Google Scholar
  33. 33.
    Dračínský M, Bouř P (2010) J Chem Theory Comput 6:288CrossRefGoogle Scholar
  34. 34.
    Franco m, Araki K, Rocha RC, et al (2000) J Solut Chem 29:667Google Scholar
  35. 35.
    Albertino A, Barge A, Cravotto G et al (2009) Food Chem 112:715CrossRefGoogle Scholar
  36. 36.
    Davison A, Jones AG (1982) Int J Appl Radiat Isot 33:875CrossRefGoogle Scholar
  37. 37.
    Spies H, Johannsen B (1981) Inorg Chim Acta 48:255CrossRefGoogle Scholar
  38. 38.
    Gottlieb HE, Kotlyar V, Nudelman A (1997) J Org Chem 62:7512CrossRefGoogle Scholar
  39. 39.
    McCleverty JA, Meyer TJ (2005) Comprehensive coordination chemistry ii, volume 5, transition metal groups 7 and 8. Elsevier, Oxford, ISBN-0-08-043748-6Google Scholar
  40. 40.
    Jacobsen NE (2007) NMR spectroscopy explained. Wiley, New Jersey, ISBN-978-0-471-73096-5Google Scholar

Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2012

Authors and Affiliations

  • R. Staník
    • 1
  • I. Benkovský
    • 1
  • J. Světlík
    • 1
  • J. Galba
    • 1
  • N. Prónayová
    • 2
  • J. Karlovská
    • 3
  1. 1.Department of Pharmaceutical Analysis and Nuclear Pharmacy, Faculty of PharmacyComenius UniversityBratislavaSlovakia
  2. 2.Department of NMR Spectroscopy, Faculty of Chemical and Food Technology, Central LaboratoriesSlovak University of TechnologyBratislavaSlovakia
  3. 3.Department of Physical Chemistry of Drugs, Faculty of PharmacyComenius UniversityBratislavaSlovakia

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