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

Marine Drugs

Mar໚ Garc໚-Altares¹  Alexis Casanova¹  Vaishali Bane²  Jorge Diogène¹  Ambrose Furey² 

[1] Institute of Agrifood Research and Technology (IRTA), Poble Nou Road, km. 5.5, Sant Carles de la Ràpita 43540, Spain; E-Mails:;Mass Spectrometry Research Centre (MSRC) and PROTEOBIO Research Group, Department of Chemistry, Cork Institute of Technology, Bishopstown, Cork, Ireland; E-Mails:

关键词: spirolides;    pinnatoxins;    Mediterranean Sea;    triple quadrupole mass spectrometry;    high resolution mass spectrometry;    orbitrap FT-MS;   

DOI  :  10.3390/md12063706

来源: mdpi

【 摘 要 】

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.

【 授权许可】

CC BY   
© 2014 by the authors; licensee MDPI, Basel, Switzerland.