title: Hydrophilic interaction liquid chromatography/mass spectrometry for determination of domoic acid in Adriatic shellfish.
abstract: This paper describes a new method for sensitive, specific and direct determination of domoic acid (DA), the causative toxin of amnesic shellfish poisoning (ASP) syndrome, in shellfish. It is based on combination of hydrophilic interaction liquid chromatography with mass spectrometry (HILIC/MS). The high percentage of organic modifier in the mobile phase and the omission of ion-pairing reagents, both favoured in HILIC, result in enhanced detection limits with MS detection. The new method was set up either on an ionspray ion trap MS instrument operating in MS and MS/MS scanning acquisition modes, or on a turboionspray triple-quadrupole MS system operating in selected ion monitoring (SIM) and multiple reaction monitoring (MRM) acquisition modes. Positive and negative ion experiments were performed. MRM experiments are recommended for screening contaminated shellfish tissue and for quantitative analyses due to highest sensitivity and selectivity. The minimum detection levels for the toxin in tissue were found to be 63 and 190 ng/g in positive and negative MRM experiments, respectively, which are well below the regulatory limit for DA in tissue (20 microg/g). Application to shellfish samples collected in the Adriatic Sea (Italy) in the period 2000-2004 demonstrated for the first time in Italy the presence of DA as a new toxin that has entered the Adriatic Mytilus galloprovincialis toxin profile.
authors.affiliation: Dipartimento di Chimica delle Sostanze Naturali, Università degli Studi di Napoli Federico II, via D. Montesano 49, 80131 Napoli, Italy.
authors.forename: Patrizia
authors.initials: P
authors.lastname: Ciminiello
authors.forename: Carmela
authors.initials: C
authors.lastname: Dell'Aversano
authors.forename: Ernesto
authors.initials: E
authors.lastname: Fattorusso
authors.forename: Martino
authors.initials: M
authors.lastname: Forino
authors.forename: Giuseppina S
authors.initials: GS
authors.lastname: Magno
authors.forename: Luciana
authors.initials: L
authors.lastname: Tartaglione
authors.forename: Michael A
authors.initials: MA
authors.lastname: Quilliam
authors.forename: Aurelia
authors.initials: A
authors.lastname: Tubaro
authors.forename: Roberto
authors.initials: R
authors.lastname: Poletti
mesh_terms: D000818:Animals; D049872:Bivalvia; D002853:Chromatography, Liquid / Q000379:methods*; D007608:Kainic Acid / Q000031:analogs & derivatives* / Q000032:analysis; D008387:Marine Toxins / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D008522:Mediterranean Sea; D012758:Shellfish; D014867:Water / Q000737:chemistry
chemical_list: D008387:Marine Toxins; D014867:Water; C012301:domoic acid; D007608:Kainic Acid