Development of a method for the identification of azaspiracid in shellfish by liquid chromatography-tandem mass spectrometry.
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.
Draisci
R
R
Laboratorio di Medicina Veterinaria, Istituto Superiore di Sanità, Rome, Italy. draisci@iss.it
Palleschi
L
L
Ferretti
E
E
Furey
A
A
James
K J
KJ
Satake
M
M
Yasumoto
T
T
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
D008387:Marine Toxins; D013141:Spiro Compounds; C406592:azaspiracid; D000095702:Polyether Toxins