Atmospheric pressure electrospray ionization mass spectra of glucose and 2-fluorodeoxyglucose for quantitative analysis of 2-fluorodeoxyglucose by high-performance liquid chromatography.
2-Fluoro-2-deoxy-D-glucose (FDG) labeled by fluorine-18 is the most widely used radiopharmaceutical for positron emission tomography (PET). For high-performance liquid chromatography (HPLC)/MS assay and quality control, the mass spectra of FDG and glucose (Glc) in organic + water solutions were studied by flow injection analysis (FIA) and in a chromatographic eluate. In acetonitrile (MeCN) + 0.025% ammonium formate (NH(4)HCO(2)) solvent (80 : 20), electrospray ionisation (ESI) of glucose-FDG provides M.NH(4)(+) and 2M.Na(+) (M = Glc or FDG) as the most intense positive ions. Formation of the latter ions and also of M.MeCN.Na(+) and 2MeCN. Na(+) is typical of the presence of NaCl in the ESI inlet. The positive ions include heavier ions corresponding to the impurities separated by HPLC and also to the cross-ring fragmentation of complexes (2FDG. aMeCNX)L, where a = 0 or 1, L is either Na(+) or NH(4)(+) and X is a fragmented pyranose or anhydropyranose residue. The second most abundant Glc negative ion is m/z = 359 which was interpreted as (2GlcH(+))(). The negative-ion spectrum of FDG has dominating lines due to FDG.HCO(2)() ions at m/z 227 and also (2FDGH(+))() at m/z 363. The m/z 363 signal is suppressed in the presence of NaCl at a molar ratio of 4 : 1 to NH(4)HCO(2), while the ions at m/z 217 and 219, i.e. FDG.Cl(), become three times more intense than FDG.HCO(2)(). The latter ion appears to be most suitable as an analytical signal for chemical analysis of FDG at m/z 226 and 227. Limits of FDG quantitation (LOQ) of 19 ng and 21 ng were found for the 200(+) and 227() ion signals, respectively, and are wholly adequate for verification of total FDG content in radiopharmaceuticals.
Department of Nuclear Chemistry, Faculty of Natural Sciences, Comenius University, SK-84215 Bratislava, Slovakia. macasek@fns.uniba.sk
F
F
Macásek
P
P
Brúder
A
A
Patakyová
E
E
Búriová
D001274:Atmospheric Pressure; D002851:Chromatography, High Pressure Liquid; D019788:Fluorodeoxyglucose F18 / Q000032:analysis / Q000737:chemistry*; D005947:Glucose / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry*; D015394:Molecular Structure; D021241:Spectrometry, Mass, Electrospray Ionization
D019788:Fluorodeoxyglucose F18; D005947:Glucose