Mass spectroscopy and chromatography of the trichloromethyl radical adduct of phenyl tert-butyl nitrone.
Positive structural identification of the PBN-trichloromethyl spin adduct in vitro was accomplished with the use of high pressure liquid chromatography and/or gas chromatography coupled with mass spectrometry. Both thin layer and liquid chromatography were used to separate a complex mixture of compounds from rat liver extracts treated with CCl4 in vitro and in vivo. Deuterated PBN's (PBN-d9; tert-butyl deuteration, or PBN-d14; both phenyl and tert-butyl deuteration) were also used to aid in the mass spectral analysis of spin adducts from liver extracts of CCl4 exposed rat livers, since the tert-butyl group fragment ion. C4D9+ (m/z = 66) is always present for PBN and PBN spin adducts. In addition, the masses of the ion peaks increase by the amount of deuteration, i.e. an increase of 9 for PBN-d9 or PBN-d14 in comparison to normally synthesized PBN.
Janzen
E G
EG
Department of Chemistry and Biochemistry, University of Guelph, Ontario, Canada.
Towner
R A
RA
Krygsman
P H
PH
Lai
E K
EK
Poyer
J L
JL
Brueggemann
G
G
McCay
P B
PB
D000818:Animals; D002251:Carbon Tetrachloride / Q000031:analogs & derivatives*; D002851:Chromatography, High Pressure Liquid; D002855:Chromatography, Thin Layer; D003497:Cyclic N-Oxides; D004578:Electron Spin Resonance Spectroscopy; D005609:Free Radicals; D008401:Gas Chromatography-Mass Spectrometry; D008862:Microsomes, Liver / Q000032:analysis; D009589:Nitrogen Oxides; D051381:Rats; D013113:Spin Labels
D003497:Cyclic N-Oxides; D005609:Free Radicals; D009589:Nitrogen Oxides; D013113:Spin Labels; C025280:trichloromethyl free radical; C029217:phenyl-N-tert-butylnitrone; D002251:Carbon Tetrachloride