title: Development of a method for the identification of azaspiracid in shellfish by liquid chromatography-tandem mass spectrometry.
abstract: Azaspiracid is the main toxin responsible for a number of recent human intoxications in Europe resulting from shellfish consumption. The first micro liquid chromatography-tandem mass spectrometry (micro-LC-MS-MS) method was developed for the determination of this novel shellfish poisoning toxin in mussels. The analyte was extracted from whole mussel meat with acetone and chromatographed on a C18 reversed-phase column (1.0 mm I.D.) by isocratic elution at 30 microl/min with acetonitrile-water (85:15, v/v), containing 0.03% trifluoroacetic acid. The toxin was ionised in an ionspray interface operating in the positive ion mode, where only the intact protonated molecule, [M+H]+, was generated at m/z 842. This served as precursor ion for collision-induced dissociation and three product ions, [M+H-nH2O]- with n=1-3, were identified for the unambiguous toxin confirmation by selected reaction monitoring LC-MS-MS analysis. A detection limit of 20 pg, based on a 3:1 signal-to-noise ratio, was achieved for the analyte. This LC-MS-MS method was successfully applied to determine azaspiracid in toxic cultivated shellfish from two regions of Ireland.
authors.affiliation: Laboratorio di Medicina Veterinaria, Istituto Superiore di Sanità, Rome, Italy. draisci@iss.it
authors.forename: R
authors.initials: R
authors.lastname: Draisci
authors.forename: L
authors.initials: L
authors.lastname: Palleschi
authors.forename: E
authors.initials: E
authors.lastname: Ferretti
authors.forename: A
authors.initials: A
authors.lastname: Furey
authors.forename: K J
authors.initials: KJ
authors.lastname: James
authors.forename: M
authors.initials: M
authors.lastname: Satake
authors.forename: T
authors.initials: T
authors.lastname: Yasumoto
mesh_terms: D000818:Animals; D049872:Bivalvia / Q000737:chemistry*; D002853:Chromatography, Liquid / Q000379:methods*; D005517:Foodborne Diseases; D008387:Marine Toxins / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013141:Spiro Compounds / Q000032:analysis*; D000095702:Polyether Toxins
chemical_list: D008387:Marine Toxins; D013141:Spiro Compounds; C406592:azaspiracid; D000095702:Polyether Toxins