A conventional high-performance liquid chromatographic (HPLC) method for the analysis of 2-fluoro-2-deoxy-d-glucose (FDG) and 2-deoxy-2-chloro-d-glucose (ClDG) in [18F]FDG preparations is described. This method was based on a postcolumn derivatization with 2-cyanoacetamide (2-CA) and UV detection. FDG and ClDG were separated on a normal-phase column using acetonitrile/water as the mobile phase. The eluate was mixed with 2-CA in sodium borate buffer solution at the outlet of a PTFE coil (10 m x 0.5 mm id) from the column, and the reaction was carried out at 100 degrees C during the passage through the coil. The UV absorbance of the resultant product was monitored at 276 nm. Under optimum conditions, the detection limits [signal-to-noise (S/N) ratio=3] for FDG and ClDG were 0.31 and 0.17 microg/ml for a 20-microl injection volume, respectively, and the linearity ranges were 0.5-100 microg/ml for both compounds. The intra- and interday reproducibilities were better than 2.2% [relative standard deviation (R.S.D.)]. This HPLC separation procedure is also useful for determining the radiochemical purity of [18F]FDG preparations since it allows the analysis of 2-[18F]fluoro-1,3,4,6-tetra-O-acetyl-d-glucose ([18F]TAG), partially hydrolyzed [18F]TAG and [18F]F-. This method can be used at many positron emission tomography (PET) facilities since it does not require an expensive, sophisticated electrochemical detector.