Potentialities of liquid chromatography with mass spectrometric detector (MSD) were investigated with the objective of quality control of radiopharmaceuticals; 2-deoxy-2-[ lsF]fluoro-D-glucose (FDG) being an example. Screening of suitable MSD analytical lines is presented. Mass-spectrometric monitoring of acetonitrile -aqueous ammonium formate eluant by negatively charged FDG.HCO 2-ions enables isotope analysis (specific activity) of the radiopharmaceutical at m/z 227 and 226. Kryptofix | 222 provides an intense MSD signal of the positive ion associated with NH4 § at m/z 394. Expired FDG injection samples contain decomposition products from which at least one labelled by 18F and characterised by signal of negative ions at m/z 207 does not correspond to FDG fragments but to C 5 decomposition products. A glucose chromatographic peak, characterised by m/z 225 negative ion is accompanied by a tail of a component giving a signal of m/z 227, which can belong to [1SO]glucose; isobaric sorbitol signals were excluded but FDG-glucose association occurs in the co-elution of separation of model mixtures. The latter can actually lead to a convoluted chromatographic peak, but the absence of 18F makes this inconsistent. Quantification and validation of the FDG component analysis is under way.