title: Confirmation of pinnatoxins and spirolides in shellfish and passive samplers from Catalonia (Spain) by liquid chromatography coupled with triple quadrupole and high-resolution hybrid tandem mass spectrometry.
abstract: Cyclic imines are lipophilic marine toxins that bioaccumulate in seafood. Their structure comprises a cyclic-imino moiety, responsible for acute neurotoxicity in mice. Cyclic imines have not been linked yet to human poisonings and are not regulated in Europe, although the European Food Safety Authority requires more data to perform a conclusive risk assessment for consumers. This work presents the first detection of pinnatoxin G (PnTX-G) in Spain and 13-desmethyl spirolide C (SPX-1) in shellfish from Catalonia (Spain, NW Mediterranean Sea). Cyclic imines were found at low concentrations (2 to 60 µg/kg) in 13 samples of mussels and oysters (22 samples analyzed). Pinnatoxin G has been also detected in 17 seawater samples (out of 34) using solid phase adsorption toxin tracking devices (0.3 to 0.9 µg/kg-resin). Pinnatoxin G and SPX-1 were confirmed with both low and high resolution (<2 ppm) mass spectrometry by comparison of the response with that from reference standards. For other analogs without reference standards, we applied a strategy combining low resolution MS with a triple quadrupole mass analyzer for a fast and reliable screening, and high resolution MS LTQ Orbitrap® for unambiguous confirmation. The advantages and limitations of using high resolution MS without reference standards were discussed.
authors: Institute of Agrifood Research and Technology (IRTA), Poble Nou Road, km. 5.5, Sant Carles de la Ràpita 43540, Spain. maria.garciaaltares@irta.cat.
authors: María
authors: M
authors: García-Altares
authors: Institute of Agrifood Research and Technology (IRTA), Poble Nou Road, km. 5.5, Sant Carles de la Ràpita 43540, Spain. alexis.casanova@irta.cat.
authors: Alexis
authors: A
authors: Casanova
authors: Mass Spectrometry Research Centre (MSRC) and PROTEOBIO Research Group, Department of Chemistry, Cork Institute of Technology, Bishopstown, Cork, Ireland. vaishali.p.bane@mycit.ie.
authors: Vaishali
authors: V
authors: Bane
authors: Institute of Agrifood Research and Technology (IRTA), Poble Nou Road, km. 5.5, Sant Carles de la Ràpita 43540, Spain. jorge.diogene@irta.cat.
authors: Jorge
authors: J
authors: Diogène
authors: Mass Spectrometry Research Centre (MSRC) and PROTEOBIO Research Group, Department of Chemistry, Cork Institute of Technology, Bishopstown, Cork, Ireland. ambrose.furey@cit.ie.
authors: Ambrose
authors: A
authors: Furey
authors: Institute of Agrifood Research and Technology (IRTA), Poble Nou Road, km. 5.5, Sant Carles de la Ràpita 43540, Spain. pablo.delaiglesia@irta.cat.
authors: Pablo
authors: P
authors: de la Iglesia
mesh_terms: D000470:Alkaloids / Q000032:analysis / Q000302:isolation & purification*; D000818:Animals; D049872:Bivalvia / Q000378:metabolism; D002853:Chromatography, Liquid / Q000379:methods*; D007097:Imines / Q000032:analysis / Q000302:isolation & purification; D008522:Mediterranean Sea; D010125:Ostreidae / Q000378:metabolism; D012015:Reference Standards; D015203:Reproducibility of Results; D012758:Shellfish; D013030:Spain; D013141:Spiro Compounds / Q000032:analysis / Q000302:isolation & purification*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000470:Alkaloids; D007097:Imines; D013141:Spiro Compounds; C552840:pinnatoxin G; C543774:spirolide I