Combined liquid chromatography/mass spectrometry of the radical adducts of a fluorescamine-derivatized nitroxide.
Dynamic liquid secondary ion mass spectrometry (dyn-LSIMS) was employed to acquire continuous, on-line mass spectral data from the effluent of a reversed-phase high-performance liquid chromatograph (HPLC) used to separate a broad suite of carbon-centered radicals trapped as the O-alkylhydroxylamine adducts of an amino nitroxide that was subsequently derivatized with fluorescamine. Data obtained by the use of these combined techniques (LC/MS) can be employed to elucidate radical adduct structures; elemental compositions of the adducts can be confirmed by acquiring mass spectra at high resolution. At low resolution, introduction into the source of < 1 pmol of adduct yielded usable spectra. The first application of this technique to the identification of photochemically generated radicals in natural water samples is presented.
Johnson
C G
CG
Department of Marine Chemistry and Geochemistry, Woods Hole Oceanographic Institution, Woods Hole, Massachusetts 02543, USA.
Caron
S
S
Blough
N V
NV
D002853:Chromatography, Liquid; D005450:Fluorescamine / Q000737:chemistry*; D005609:Free Radicals; D013058:Mass Spectrometry; D009569:Nitric Oxide / Q000737:chemistry*
D005609:Free Radicals; D009569:Nitric Oxide; D005450:Fluorescamine