Abstract: The residual solvents in PET radiopharmaceuticals were analyzed by GC, which were acetonitrile, ethanol, N,N-dimethylethanolamine(DMEA), dimethylsulfoxide (DMSO). The standard curves were established with the AT-624 capillary column at GC, and the sensitivity of cetonitrile and ethanol were 0.004～0.320 g/L and 0.010～0.120 g/L respectively. The residual solvents of acetonitrile, ethanol, DMEA and DMSO in PET radiopharmaceuticals were analyzed by GC. The linearity were 0.999 4,0.999 9, 0.999 7, 0.999 6 respectively.The residual of acetonitrile were （0.031 3±0.043 3）、（0.082 9±0.066 8）、（0.015 6±0.005 9）、（0.025 4±0.026 6） g/L in ¹⁸F-FDG, ¹⁸F-FLT, ¹¹C-CFT, ¹¹C-PIB respectively. The residual of ethanol was (0.050 5±0.005 28) g/L in ¹⁸F-FDG. The residual of DMSO were (0.033 1±0.018 0) g/L, (0.023 8±0.010 0) g/L in ¹⁸F-W372 and ¹¹C-DTBZ respectively. The residual of DMEA was (0.034 8±0.002 2) g/L in ¹¹C-Choline. The survived of organic solvent in PET radiopharmaceuticals can be analyzed with GC directly. The results showed that the QC should be done in PET radiopharmaceuticals purity with semi-HPLC to avoid the high residual.