title: Liquid chromatography-high-resolution mass spectrometry for palytoxins in mussels.
abstract: Palytoxins from Ostreopsis cf. ovata (a putative palytoxin and ovatoxins) are emerging toxins in the Mediterranean basin and are not yet regulated, although there is evidence that they can accumulate in seafood and thus enter the human food chain. This poses serious concerns for human health, because palytoxin itself is among the most potent marine toxins known. In 2009, the European Food Safety Authority (EFSA) announced the need for optimization of efficient analytical methods for detecting palytoxins and for preparing standards. Herein, we propose a procedure including a one-step extraction, solid-phase-extraction (SPE) clean-up, and liquid chromatography-high resolution mass spectrometry (LC-HRMS) detection of individual palytoxins in mussels. The method enabled efficient chromatographic separation of individual compounds, including structural isomers, with good sensitivity, reproducibility, and linearity in a large dynamic range (14-1000 ng mL(-1) in matrix). As a result, the putative palytoxin from Ostreopsis cf. ovata was identified as an isomer of palytoxin itself and re-named isobaric palytoxin. 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 μg kg(-1) in crude mussel extracts and 15 μg kg(-1) after SPE clean-up. Although full validation of the method is currently prevented by the unavailability of palytoxin(s) certified standards and reference material, this study constitutes a first step towards achieving this.
authors.affiliation: Department of Pharmacy, University of 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: Emma
authors.initials: E
authors.lastname: Dello Iacovo
authors.forename: Martino
authors.initials: M
authors.lastname: Forino
authors.forename: Luciana
authors.initials: L
authors.lastname: Tartaglione
mesh_terms: D000178:Acrylamides / Q000032:analysis*; D000818:Animals; D049872:Bivalvia / Q000737:chemistry*; D002853:Chromatography, Liquid / Q000379:methods*; D003064:Cnidarian Venoms; D005506:Food Contamination / Q000032:analysis; D059022:Food Safety; D008387:Marine Toxins / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D012758:Shellfish / Q000032:analysis*; D000095702:Polyether Toxins
chemical_list: D000178:Acrylamides; D003064:Cnidarian Venoms; D008387:Marine Toxins; C010272:palytoxin; D000095702:Polyether Toxins