Research on marine biotoxins has shown a continuously changing toxin profile in the Mediterranean area with most of the toxin classes so far known being present in seafood collected along the Italian coastline. Starting from the late ‘80s with the first finding of okadaic acid in Adriatic mussels, a number of other classes of marine toxins have been found, including yessotoxins, pectenotoxins, saxitoxins, domoic acid, spirolides, palytoxins, and azaspiracids. Liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS) presents great potential for the identification of all the above mentioned toxins as well as for the structural characterization of the unknowns, due to its high detection sensitivity and selectivity, stable mass accuracy, and large dynamic range. Some of the LC-HRMS methods and HRMSn based strategies used for gaining structural insights on the toxins of highest concern in the Mediterranean area are presented. A special focus is given to palytoxins, emerging toxins which are not regulated yet although there is evidence that they can accumulate in seafood thus entering the human food chain. A procedure including a one-step extraction, solid phase extraction (SPE) clean-up and LC-HRMS detection of individual palytoxins in mussels has been developed. The instrumental method allows an efficient chromatographic separation of individual compounds, including structural isomers, with good sensitivity, reproducibility and linearity in the range 14-1000 ng/mL in matrix. The whole procedure (sample preparation and LC-HRMS analysis) proved able to detect palytoxins in both spiked and natural mussel samples at levels as low as 70 ug/kg in crude mussel extracts and 15 ug/kg after SPE clean-up, well below the maximum level of 30 ug/kg suggested by EFSA. Although a full validation of the method is currently prevented by the unavailability of palytoxin(s) certified standards and reference material, this study constitutes the first unavoidable step in such a direction.
High-Resolution Orbitrap Mass Spectrometry for the Identification of the Emerging Threats to Seafood Consumers in the Mediterranean Area / Dell'Aversano, Carmela; Tartaglione, Luciana. - (2017). (Intervento presentato al convegno SEAFOOD SAFETY NEW FINDINGS & INNOVATION CHALLENGES INTERNATIONAL STAKEHOLDER EVENT & OPEN SCIENCE CONFERENCE tenutosi a Royal Flemish Academy of Science and the Arts (KVAB), Brussels, Belgium nel 25-26 January 2017).
High-Resolution Orbitrap Mass Spectrometry for the Identification of the Emerging Threats to Seafood Consumers in the Mediterranean Area
DELL'AVERSANO, CARMELA;TARTAGLIONE, LUCIANA
2017
Abstract
Research on marine biotoxins has shown a continuously changing toxin profile in the Mediterranean area with most of the toxin classes so far known being present in seafood collected along the Italian coastline. Starting from the late ‘80s with the first finding of okadaic acid in Adriatic mussels, a number of other classes of marine toxins have been found, including yessotoxins, pectenotoxins, saxitoxins, domoic acid, spirolides, palytoxins, and azaspiracids. Liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS) presents great potential for the identification of all the above mentioned toxins as well as for the structural characterization of the unknowns, due to its high detection sensitivity and selectivity, stable mass accuracy, and large dynamic range. Some of the LC-HRMS methods and HRMSn based strategies used for gaining structural insights on the toxins of highest concern in the Mediterranean area are presented. A special focus is given to palytoxins, emerging toxins which are not regulated yet although there is evidence that they can accumulate in seafood thus entering the human food chain. A procedure including a one-step extraction, solid phase extraction (SPE) clean-up and LC-HRMS detection of individual palytoxins in mussels has been developed. The instrumental method allows an efficient chromatographic separation of individual compounds, including structural isomers, with good sensitivity, reproducibility and linearity in the range 14-1000 ng/mL in matrix. The whole procedure (sample preparation and LC-HRMS analysis) proved able to detect palytoxins in both spiked and natural mussel samples at levels as low as 70 ug/kg in crude mussel extracts and 15 ug/kg after SPE clean-up, well below the maximum level of 30 ug/kg suggested by EFSA. Although a full validation of the method is currently prevented by the unavailability of palytoxin(s) certified standards and reference material, this study constitutes the first unavoidable step in such a direction.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
