Determination of azide in gastric fluid and urine by flow-injection electrospray ionization tandem mass spectrometry

• Minakata, Kayoko

• Nozawa, Hideki

• Yamagishi, Itaru

• Gonmori, Kunio

• Hasegawa, Koutaro

• Suzuki, Masako

• Watanabe, Kanako

• Suzuki, Osamu

Abstract

application/pdf

A rapid method was developed to identify and quantify the azide ion (N3?) in gastric fluid and urine. N3? in diluted biological fluids was reacted with NaAuCl4 to produce Au(N3)2?, which was extracted with octanol. Five microliters of the extract were flow-injected into an electrospray ionization tandem mass spectrometric instrument. Quantification of N3? was performed by selected reaction monitoring of the product ion Au(N)(N3) ? at m/z 253 which was derived from the precursor ion Au(N3)2? at m/z 281, using 50 μL of aqueous solution within 10 min. This method was found to be linear up to 10?5 M, to have a limit of quantification of 10?7 M, a limit of detection of 3.0×10?8 M, and a coefficient of variation of ≦ 10 % at 10?7 M. In case of urine, 50 μL of urine were spiked with N3?, this was diluted to10-fold and passed through 1 mL of a resin and finally diluted to 100-fold of the original. This method was linear up to 10?3 M, had a limit of quantification of 10?5 M, a limit of detection of 3.0×10?6 M, and coefficient of variation ≦ 8.8 % for an original urine concentration of 10?5 M. The practical applicability of this method was checked by diluting 1 μL of a suspected suicide victim’s gastric fluid 20,000-fold and 1 μL of the victim’s urine 5,000-fold and then measuring the N3? levels. These levels were found to be (7.5±1.0)×10?2 M and (3.2±0.4)×10?3 M, respectively.

Journal

• Analytical and Bioanalytical Chemistry

  Analytical and Bioanalytical Chemistry 403 (7), 1793-1799, 2012-06

  Springer

Keywords

• Azide
• Gold
• Electrospray ionization
• Tandem mass spectrometry
• Gastric fluid
• Urine

Details

• CRID: 1050282676653063168
• NII Article ID: 120005671500
• DOI: 10.1007/s00216-012-5848-3
• ISSN: 16182650
• ISSN: 16182642
• HANDLE: 10271/2908
• Web Site: https://hama-med.repo.nii.ac.jp/records/2770
• Web Site: http://link.springer.com/content/pdf/10.1007/s00216-012-5848-3.pdf
• Web Site: http://link.springer.com/article/10.1007/s00216-012-5848-3/fulltext.html
• Web Site: http://link.springer.com/content/pdf/10.1007/s00216-012-5848-3
• Text Lang: en
• Article Type: journal article
• Data Source:
  • IRDB
  • Crossref
  • CiNii Articles
  • KAKEN