A 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

During the investigation of aviation accidents, postmortem samples from victims are submitted to the Federal Aviation Administration's Civil Aerospace Medical Institute (CAMI) for drug analysis. Because new drugs are continually being released, CAMI must develop methods to 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 but it does have certain side effects that could create potential hazards. The procedure described herein incorporates solid-phase extraction and liquid chromatograph (LC)/mass spectrometer (MS)/MS and MS/MS/MS utilizing an atmospheric pressure chemical ionization ion trap mass spectrometer in the positive ionization 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 intra-day (within day) relative error of equal to or less than 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 equal to or less than 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 4C. 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.

• Record URL:
  http://www.faa.gov/data_research/research/med_humanfacs/oamtechreports/2000s/media/00_20.pdf
• 
• Corporate Authors:

  Federal Aviation Administration

  Civil Aerospace Medical Institute, P.O. Box 25082
  Oklahoma City, OK  United States  73125

  University of Oklahoma, Norman

  Department of Chemistry and Biochemistry
  Norman, OK  United States  73069
• Authors:
  • Lewis, R L
  • Johnson, R D
  • Blank, C L
• Publication Date: 2000-5

Language

• English

Media Info

• Features: Figures; References; Tables;
• Pagination: 15 p.

Subject/Index Terms

• TRT Terms: Aircraft crash victims; Aviation medicine; Crash investigation; Forensic medicine; Laboratory tests; Liquid chromatography; Mass spectrometry; Medication; Specimens; Test procedures
• Identifier Terms: Civil Aeromedical Institute; U.S. Federal Aviation Administration
• Uncontrolled Terms: Sildenafil
• Subject Areas: Aviation; Safety and Human Factors;

Filing Info

• Accession Number: 00929924
• Record Type: Publication
• Report/Paper Numbers: DOT/FAA/AM-00/20
• Files: TRIS, USDOT
• Created Date: Aug 12 2002 12:00AM