A method to determine tetrodotoxin (TTX) in globefish by solid phase extractions and gas chromatography mass spectrometry (GC-MS) is described. TTX in globefish sample was extracted with 2% acetic acid/methanol, defatted by petroleum ether, evaporated to dryness under reduced pressure. Then the compound was converted to 2 amino 6 hydroxymethyl 8 hydroxyquinazoline (C9 base) under alkaline conditions and extracted by use of an MCX extraction cartridge. The C9 base was analyzed after trimethylsilyl derivation (TMS) C9 base by GC-MS scan mode, the qualified ions are 376, 392, 407. (TMS) C9 base is quantified by GC-MS selected ion monitoring. The quantified ion was 392. The calibration curve was linear in the range of 0.05-5.0 μg /mL and linear relationship R²=0.997 5. For the 0.02,0.1,0.5 mg/kg spiked samples , the recovery rate were 64.0%-92.8%, RSDs were 5.41%-8.63% for six times, and the limitation of quantification was 5.0 μg/kg. From the results of above, detection of TTX in aquatic products by solid phase extractions and gas chromatography/mass spectrometry (GC MS) is sensitive, accurate and feasible.