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A method to determine tetrodotoxin (TTX) in human plasma by solid-phase extractions and gas chromatography/mass spectrometry (GC/MS) is described. TTX in plasma samples was passed through Sep-Pak PS-2 extraction cartridges, Then the compound was converted to 2-amino-6-hydroxymethyl-8-hydroxyquinazoline (C9-base) under alkaline conditions and extracted with use of an OASIS HLB extraction cartridge. The C9-base was analyzed after trimethylsilyl derivatization by GC/MS-selected ion monitoring. Recovery rates were 35.3-50.8% and their coefficients of variation were not greater than 16.6%. The calibration curve was linear in the range of 0.5-10.0 ng ml(-1) and the detection limit was 0.1 ng ml(-1). The coefficients of within-day and day-to-day variations were not greater than 11.8%. Actual determination of TTX in rat plasma after intraperitoneal administration was also presented.