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Hydrophilic interaction liquid chromatography/mass spectrometry for determination of domoic acid in Adriatic shellfish
Author(s) -
Ciminiello Patrizia,
Dell'Aversano Carmela,
Fattorusso Ernesto,
Forino Martino,
Magno Giuseppina S.,
Tartaglione Luciana,
Quilliam Michael A.,
Tubaro Aurelia,
Poletti Roberto
Publication year - 2005
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.2021
Subject(s) - domoic acid , chemistry , chromatography , hydrophilic interaction chromatography , detection limit , shellfish , mass spectrometry , marine toxin , shellfish poisoning , selected reaction monitoring , triple quadrupole mass spectrometer , ion trap , paralytic shellfish poisoning , liquid chromatography–mass spectrometry , toxin , high performance liquid chromatography , tandem mass spectrometry , fish <actinopterygii> , fishery , aquatic animal , biochemistry , biology
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 µg/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. Copyright © 2005 John Wiley & Sons, Ltd.