Mass Spectrometry Letters

Korean Society for Mass Spectrometry (한국질량분석학회)
권호 표지
DOI QR코드

DOI QR Code

Determination of the PDE-5 Inhibitors and Their Analogues by GC-MS and TMS Derivatization

  • Pyo, Jae-Sung (Southern District Office of National Forensic Service) ;
  • Lee, Hee-Sang (Southern District Office of National Forensic Service) ;
  • Park, Yu-Jin (Southern District Office of National Forensic Service) ;
  • Jo, Ji-Yeong (Southern District Office of National Forensic Service) ;
  • Park, Yong-Hoon (Southern District Office of National Forensic Service) ;
  • Choe, Sang-Gil (Southern District Office of National Forensic Service) ;
  • Lee, Mi-Young (Industrial Safety and Health Research Institute) ;
  • Lee, Jae-Sin (Narcotics Analysis Division of National Forensic Service)
  • Received : 2011.05.02
  • Accepted : 2012.02.23
  • Published : 2012.03.15

Abstract

Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could be identified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil and mirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.

Keywords

File

Download PDF

References

  1. Reffelmann, T.; Kloner, R. A. Curr. Pharm. Des. 2006, 12, 3485. https://doi.org/10.2174/138161206778343073
  2. Gorge, G.; Flüchter, S.; Kirstein, M.; Kunz, T. Herz 2003, 28, 284. https://doi.org/10.1007/s00059-003-2478-8
  3. Nagaraju, V.; Sreenath, D.; Rao, J. T.; Rao, R. N. Anal. Sci. 2003, 19, 1007. https://doi.org/10.2116/analsci.19.1007
  4. Choi, D. M.; Park, S. A.; Yoon, T. H.; Jeong, H. K.; Pyo, J. S.; Park, J. H.; Kim, D. J.; Kwon, S. W. J. AOAC Int. 2008, 91, 580.
  5. Reepmeyer, J. C.; Woodruff, J. T.; d'Avignon, D. A. J. Pharm. Biomed. Anal. 2007, 43, 1615. https://doi.org/10.1016/j.jpba.2006.11.037
  6. Man, C. N.; Nor, N. M.; Lajis, R.; Harn, G. L. J. Chromatogr. A 2009, 1216, 8426. https://doi.org/10.1016/j.chroma.2009.10.016
  7. Instrumental Analysis Data of Illegal Compounds in Food, National Institute of Food and Drug Safety Evaluation of Korea, Seoul, 2010.
  8. Saisho, K.; Scott, K. S.; Morimoto, S.; Nakahara, Y. Biol. Pharm. Bull. 2001, 24, 1384. https://doi.org/10.1248/bpb.24.1384
  9. Riddick, L.; Gentry, E. L.; McDaniel, M.; Brumley, W. C. Int. J. Environ. Anal. Chem. 2006, 86, 299. https://doi.org/10.1080/03067310500211294

Cited by

  1. Detection and structure elucidation of hydroxythiovardenafil as an adulterant in a herbal dietary supplement vol.74, 2013, https://doi.org/10.1016/j.jpba.2012.10.013
  2. Rapid determination of sildenafil and its analogues in dietary supplements using gas chromatography–triple quadrupole mass spectrometry vol.121, 2016, https://doi.org/10.1016/j.jpba.2016.01.034
  3. Simultaneous Determination of Synthetic Phosphodiesterase-5 Inhibitors in Dietary Supplements by Liquid Chromatography-High Resolution/Mass Spectrometry vol.3, pp.2, 2012, https://doi.org/10.5478/MSL.2012.3.2.50