A novel approach to the analysis of spin-trapped free radicals using dimethyl sulfoxide and gas chromatography - mass spectrometry (GC-MS) with both solvent extraction and headspace solid phase microextraction (HS-SPME).

In this study, we have utilized a novel strategy based upon the use of dimethyl sulfoxide (DMSO) and gas chromatography-mass spectrometry (GC-MS) for the detection and identification of spin-trapped free radicals. Hydroxymethyl (CHOH) radicals, generated by Fenton-type chemistry, have been trapped by --butyl-α-phenylnitrone (PBN) or one of its derivatives in the presence of DMSO to form a 1,3-diadduct [PBN-(CHOH)(CH)], which may be detected directly in the reaction mixture following chloroform extraction or in the reaction vial headspace by sampling with SPME. Separation and identification have been carried out by capillary gas chromatography coupled to electron-ionization mass spectrometry (EI-MS).