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XXXV TIAFT Annual Meeting Poster Presentations
GC/MS ANALYSIS OF URINARY HIPPURIC ACID USING SIMPLE SAMPLE PREPARATION

Hara K., Kashimura S., Morinaga M., Kageura M.

Department of Forensic Medicine, Fukuoka University School of Medicine, Nanakuma, Fukuoka, Japan

An exctractive heptafluoro-n-butyrylation on Extrelut column has been developed for simultaneously, simply and rapidly determining methamphetamine and its metabolites in biological materials. The aim of this study was to apply the method to detecting urinary hippuric acid in touluene-abusers.
Methods. For a regular preparation, 0.1 mL of urine was diluted with 6 mL of 0.01 M HCl. An 1 mL aliquot of the diluted urine was spiked with N-benzoyl-L-alanine as an internal standard (IS). After pH adjustment to 12.6, the solution was applied onto an Extrelut column. After 15 min, the analyte was eluted with n-hexane including 1% heptafluoro-n-butyryl chloride. Following the condensation under a gentle nitrogen stream, the extract was diluted with ethyl acetate and analyzed by GC/MS.
Results. The mass spectrum corresponding to hippuric acid indicated the principal ions at m/z 161 (molecular ion: C9H7NO2), m/z 117, m/z 105, m/z 77 (base peak ion). Its precursor compound indicating the molecular ion at m/z 357 (the heptafluoro-n-butyrylated form), was observed in a small peak. The resulting compound was estimated as 1,2,3,4-tetrahydro-1,4-dioxo-2-isoquinoline. Meanwhile the mass spectrum of IS possessed the main ions at m/z 175 (molecular ion), m/z 131, m/z 105, m/z 77. Each peak was distinguishable on the base line level. The linearity was observed in a range from 0.83 µg to 83.3 µg. The day-to-day precision was satisfactory within 10% in coefficients of variation. By adding methamphetamine-d5 and 4-hydroxymethamphetamine-d5 as Iss, also, methamphetamine and its main metabolites could be quantitatively detected.
Conclusion. By using this method, two forensic toxicological tests for demonstrating methamphetamine-abuse and toluene-exposure can be simultaneously performed.

  Abstract 146

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