Novel Method for the Determination of Sildenafil (Viagra) and Its Metabolite (UK-103,320) in Postmortem Specimens Using LC/MS/MS and LC/MS/MS/MS.

Details

• Creators:
  Lewis, R. J. ; Johnson, R. D. ; Blank, C. L.
• Corporate Contributors:
  United States. Department of Transportation. Federal Aviation Administration. Civil Aerospace Medical Institute ; University of Oklahoma. Dept. of Chemistry and Biochemistry ; United States. Office of Aviation Medicine
• Subject/TRT Terms:
  • Fatalities
  • Air transportation crashes
  • Drug use
  • Drugs
  • Drug effects
  • Autopsy
  • Aviation accidents
  • Death
  • Drug analysis
  • Metabolites
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• Publication/ Report Number:
  DOT/FAA/AM-00/20
• Resource Type:
  Research Paper
• Geographical Coverage:
  United States
• Corporate Publisher:
  United States. Federal Aviation Administration. Office of Aviation Medicine
• Abstract:
  During the investigation of aviation accidents, postmortem samples from victims are submitted to the FAA’s ; Civil Aeromedical Institute for drug analysis. Because new drugs are continually being released to the market, it ; is our laboratory’s responsibility to develop methods which can identify these new drugs. This paper presents a ; rapid and reliable method for the identification and quantitation of sildenafil (Viagra®) and its metabolite, UK- ; 103,320. Sildenafil, when used properly, is relatively safe. There are, however, certain side effects that could ; create potential hazards. For example, Sildenafil has been shown to potentiate the hypotensive effects of nitrates ; commonly employed in the treatment of certain heart conditions. The procedure described herein incorporates ; solid-phase extraction and LC/MS/MS and MS/MS/MS utilizing an atmospheric pressure chemical ionization ; (APCI) ion trap mass spectrometer (MS) in the positive ionization (PCI) mode. Solid-phase extraction provided ; an efficient sample extraction yielding recoveries of approximately 80%. This method is highly selective and ; sensitive, having a limit of detection of 1 ng/mL for both compounds. Sildenafil and UK-103,320 were found ; to have a linear dynamic range of 2-800 ng/mL and 4-800 ng/mL, respectively. This procedure showed intraday ; (within day) relative error of £ 6% and relative standard deviation (RSD) within 4% for both the 50 ng/mL ; and 200 ng/mL controls. The inter-day (between day) relative errors were £ 4%, while the RSD was within ; 12% for both control concentrations. Sildenafil and UK-103,320 were found to be stable in blood for at least ; one week at 4°C. This method was also used for the determination of sildenafil and UK-103,320 in postmortem ; fluid and tissue specimens collected from fatal aviation accident victims.
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• Format:
  PDF
• Download URL:
  https://rosap.ntl.bts.gov/view/dot/15398/dot_15398_DS1.pdf
• File Type:
  [PDF - 240.90 KB]
• Collection(s):
  US Transportation Collection ; FAA Civil Aerospace Medical Institute
• Main Document Checksum:
  urn:sha-512:7d01ecad79da732b87b8c95524ed7d9da997ff1f6408adfbd1d5db3d1b11edebe3bd12a46b163adbba31b03728f989bb3d2c17df384125b6a163a70a8b0f7479