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Enhanced recognition of spin trapped radicals in complex mixtures: Deuterated nitronyl adducts provide a gas chromatographic/mass spectrometric marker

Journal Article · · Analytical Letters; (USA)
The use of deuterated analogues of {alpha}-phenyl-N-tert-butyl nitrone (PBN) are reported for GC/MS analysis of spin trapping products. PBN-d{sub 9} and PBN-d{sub 14}, deuterated in the tert-butyl group (the latter also deuterated in the phenyl ring), result in a more diagnostic fragment ion, C{sub 4}D{sub 9}{sup +} (m/z = 66) which improves the recognition of PBN adducts in mixtures. This feature has helped identify a new 1,3-radical addition product of PBN-d{sub 9} formed during azobis(isobutyronitrile) thermolysis (addition of 2-cyano-2-propyloxyl followed by 2-cyano-2-propyl radicals). The {sup 13}C-trichloromethyl radical adduct of PBN-d{sub 14} produced during {sup 13}C-carbon tetrachloride incubation with rat liver microsomes was identified by GC/MS in a complicated biological extract mixture. 25 refs., 3 figs., 1 tab.
OSTI ID:
5143956
Journal Information:
Analytical Letters; (USA), Journal Name: Analytical Letters; (USA) Vol. 22:4; ISSN ANALB; ISSN 0003-2719
Country of Publication:
United States
Language:
English