title: [Analysis of tetrodotoxin in puffer-fish by LC/MS].
abstract: A simple and reliable method using liquid chromatography/electrospray ionization-mass spectrometry (LC/ESI-MS) for the analysis of tetrodotoxin in puffer-fish was developed. Tetrodotoxin in puffer-fish was extracted with 0.1% acetic acid by heating in a boiling water bath, and the extracts were cleaned up on a Bond Elut C18 (500 mg) cartridge. The LC separation was performed on a TSK-gel ODS 80Ts column (25 cm x 2 mm i.d.) using 5 mmol/L heptafluoro-n-butyric acid (HFBA)-methanol (99:1) as the mobile phase at a flow rate of 0.2 mL/min. Positive ionization produced a typical [M + H]+ molecular ion of tetrodotoxin (m/z 320.1). The calibration graph for tetrodotoxin was rectilinear from 0.1 to 1 microgram/mL with selected ion monitoring (SIM). The detection limit of tetrodotoxin in puffer-fish was 1 microgram/g (equivalent to ca. 5 MU/g).
authors.affiliation: Saitama Prefectural Institute of Public Health: 639-1, Kamiokubo, Saitama, Saitama 338-0824, Japan.
authors.forename: Masakazu
authors.initials: M
authors.lastname: Horie
authors.forename: Rie
authors.initials: R
authors.lastname: Ishii
authors.forename: Susumu
authors.initials: S
authors.lastname: Kobayashi
authors.forename: Hiroyuki
authors.initials: H
authors.lastname: Nakazawa
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods; D013058:Mass Spectrometry / Q000379:methods; D023721:Tetraodontiformes / Q000378:metabolism*; D013779:Tetrodotoxin / Q000032:analysis*
chemical_list: D013779:Tetrodotoxin