title: Mass spectroscopy and chromatography of the trichloromethyl radical adduct of phenyl tert-butyl nitrone.
abstract: 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.
authors.affiliation: Department of Chemistry and Biochemistry, University of Guelph, Ontario, Canada.
authors.forename: E G
authors.initials: EG
authors.lastname: Janzen
authors.forename: R A
authors.initials: RA
authors.lastname: Towner
authors.forename: P H
authors.initials: PH
authors.lastname: Krygsman
authors.forename: E K
authors.initials: EK
authors.lastname: Lai
authors.forename: J L
authors.initials: JL
authors.lastname: Poyer
authors.forename: G
authors.initials: G
authors.lastname: Brueggemann
authors.forename: P B
authors.initials: PB
authors.lastname: McCay
mesh_terms: 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
chemical_list: 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