title: Palytoxin in seafood by liquid chromatography tandem mass spectrometry: investigation of extraction efficiency and matrix effect.
abstract: Blooms of Ostreopsis spp. have been recently reported along the Mediterranean coasts of Spain, France, Italy, and Greece posing serious risks to human health. Occurrence of Ostreopsis spp. may result in palytoxin contamination of seafood and, in order to prevent sanitary risks, the need exists to develop efficient extraction procedures to be coupled to rapid and sensitive monitoring methods of palytoxin-like compounds in seafood. In the present study, the best conditions for both extraction of palytoxin from seafood and palytoxin quantification by using liquid chromatography tandem mass spectrometry (LC-MS/MS) were investigated. Three seafood matrices (mussels, sea-urchins, and anchovies) were selected and five different extraction systems were tested, namely: the official protocol for extraction of lipophilic toxins and various aqueous methanol or acetonitrile solutions (MeOH/H(2)O 1:1, MeOH/H(2)O 8:2, MeCN/H(2)O 8:2 and MeOH 100%). Extraction with MeOH/H(2)O 8:2 provided the best results in terms of accuracy and matrix interference on LC-MS/MS detection of palytoxin. Accuracy and intra-day reproducibility (n = 3) were evaluated for all the selected matrices but only for mussels at three spiking concentration levels, including the provisional limit proposed by the Community Reference Laboratory for marine biotoxins (250 μg kg(-1)). Limits of quantitation of palytoxin in mussels, sea-urchins and anchovies tissues were calculated using matrix-matched standards; taking into account extraction efficiency of MeOH/H(2)O 8:2, they resulted to be 228, 343, and 500 μg kg(-1), respectively.
authors.affiliation: Dipartimento di Chimica delle Sostanze Naturali, Università degli Studi di Napoli Federico II, via D. Montesano 49, 80131 Naples, 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: Ernesto
authors.initials: E
authors.lastname: Fattorusso
authors.forename: Martino
authors.initials: M
authors.lastname: Forino
authors.forename: Luciana
authors.initials: L
authors.lastname: Tartaglione
authors.forename: Rachele
authors.initials: R
authors.lastname: Rossi
authors.forename: Vittorio
authors.initials: V
authors.lastname: Soprano
authors.forename: Daniela
authors.initials: D
authors.lastname: Capozzo
authors.forename: Luigi
authors.initials: L
authors.lastname: Serpe
mesh_terms: D000178:Acrylamides / Q000032:analysis*; D000818:Animals; D049872:Bivalvia / Q000737:chemistry; D019086:Bridged Bicyclo Compounds, Heterocyclic / Q000032:analysis; D002853:Chromatography, Liquid; D003064:Cnidarian Venoms; D005506:Food Contamination / Q000032:analysis*; D005524:Food Technology / Q000379:methods*; D005602:France; D007558:Italy; D057230:Limit of Detection; D008387:Marine Toxins / Q000032:analysis; D015394:Molecular Structure; D011714:Pyrans / Q000032:analysis; D015203:Reproducibility of Results; D012617:Sea Urchins / Q000737:chemistry; D017747:Seafood / Q000032:analysis*; D013030:Spain; D053719:Tandem Mass Spectrometry; D000095702:Polyether Toxins
chemical_list: D000178:Acrylamides; D019086:Bridged Bicyclo Compounds, Heterocyclic; D003064:Cnidarian Venoms; D008387:Marine Toxins; D011714:Pyrans; C010272:palytoxin; D000095702:Polyether Toxins; C459585:ostreocin D