Analysis of Sildenafil and its Analogues by LC/MS/MS

LC/MS/MS를 이용한 sildenafil 및 그 유사체 분석

  • Myung, Seung-Woon (Doping Control Center, Korea Institute of Science and Technology) ;
  • Park, So-Hee (Doping Control Center, Korea Institute of Science and Technology) ;
  • Cho, Hyun-Woo (Department of Chemistry, KyongGi University)
  • 명승운 (한국과학기술연구원 도핑콘트롤센터) ;
  • 박서희 (한국과학기술연구원 도핑콘트롤센터) ;
  • 조현우 (경기대학교 이과대학 화학과)
  • Received : 2003.08.07
  • Accepted : 2003.10.16
  • Published : 2003.12.25


By LC/MS/MS, the analytical method of sildenafil and its analogues (homosildenafil, vardenafil and tadalafil) used as used medical treatment of impotence was established. electrosprary ionization (ESI) and atmospheric pressure chemical ionization (APCI) as a ionization method were applied. Several parameter were varied and the sensitivity and reproducibility were compared. In LC/ESI-MS method, capillary voltage, cone voltage, extractor, entrance and RF lens to create appropriate productr ions for multiple reaction monitoring (MRM) were variable parameter, but the formation of the other product ions except the precursor ion could not detect. And the value of entrance, collision energy, exit, corona voltage, cone voltage, extractor, RF lens, cone gas, and desolvation gas in APCI mode were varied, only the creation pattern of fragment ions by the change of RF lens value were detected, and the limit of detection was decreased due to the increase of S/N. Ten millimole ammonium formate (pH 4.8):acetonitrile=70:30 by isocratic elution in HPLC system was shown the maximum sensitivity in MS, the detection limit of sildenafil, homosildenafil, vardenafil and tadalafil obtained by ESI-MRM were 0.10, 0.025, 0.025, and $0.25{\mu}g/mL$ at S/N>5, respectively.


  1. Graham N. MAw, Charlotte M. N. Allerton, Eugene Gbekor, William A. Million, Bioorganic & Medicinal Chemistry Letters, 13, 1425-1428(2003).
  2. J. D. H. Cooper, D. C. Muirhead, J. E. Taylor, R. T. Baker, J. Chromatogr. B, 701, 87-95(1997).
  3. C. K. Jeong, H. Y. Lee, M. S. Jang, W. B. Kim, H. S. Lee, J. Chromatogr. B,752, 141-147(2001).
  4. W. Weinmann, M. Bohnert, A. Wiedemann, M. Renz, N. Lehmann, S. Pollak, Int. J. Legal Med., 114, 252-258(2001)
  5. V. Dumesrre-Toulet, V. Cifimele, S. Gromb, T. Beloussoff, Lavault, B. Ludes, P. Kintz, Forensic Sci. Int. 126, 71-76(2002).
  6. Angela Eerkes, Tom Addison, Weng Naidong, J. Chromatography B, 768, 277-284(2002).
  7. H. Porst, H. Padma-Nathan, F. Giuliano, G. Anglin, L. Varanese, R. Rosen, Urology, 62, 121-125(2003).
  8. A. Eerkes. T. Addision. T.A ddison, W. Naidoge, J. Chromatogr. B 768, 277-284(2002).
  9. R. Hyland, E. G. H. Roe, B. C Jones, D. A. Smith, Br. J. Clin. Pharmacal., 51, 239-248(2000).
  10. J. Kim, H. Y. Ji S. Kim, H. W. Lee, S.-S. Lee, D. S. Kim, M. Yoo, W. B. Kim, H. S. Lee, J. Pharmaceutical and Biomedical Analysis, 32, 317-322(2003).
  11. J. J. B. Nevado, J. R. Flores, G. C. Penalvo, N. R. Farinas, J. Chromatogr. A, 953, 279-286(2002).
  12. K. Saisho, K. S. Scott, S. Morimoto, Y. Nakahara, BioI. Pharm. Bull, 24, 1384-1388(2001).
  13. c.-S. Lin, Z.-c. Xin, G. Lin, T. F. Lue, Urology, 61, 685-691(2003).
  14. 김택제, 명승운, 조현우, 김명수, '실용적인 기체.액체 크로마토그래피와 질량분석법', 353-367, 자유 아카데미, 2002.
  15. J. Law, T. W. Chang, J. Chromatogr. B, 765, 161-166(2001).