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Mar. Drugs 2014, 12(6), 3706-3732; doi:10.3390/md12063706
Article

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

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Received: 4 April 2014; in revised form: 13 May 2014 / Accepted: 19 May 2014 / Published: 23 June 2014
(This article belongs to the Special Issue Emerging Marine Toxins)
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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.
Keywords: spirolides; pinnatoxins; Mediterranean Sea; triple quadrupole mass spectrometry; high resolution mass spectrometry; orbitrap FT-MS spirolides; pinnatoxins; Mediterranean Sea; triple quadrupole mass spectrometry; high resolution mass spectrometry; orbitrap FT-MS
This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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MDPI and ACS Style

García-Altares, M.; Casanova, A.; Bane, V.; Diogène, J.; Furey, A.; de la Iglesia, P. 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. Mar. Drugs 2014, 12, 3706-3732.

AMA Style

García-Altares M, Casanova A, Bane V, Diogène J, Furey A, de la Iglesia P. 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. 2014; 12(6):3706-3732.

Chicago/Turabian Style

García-Altares, María; Casanova, Alexis; Bane, Vaishali; Diogène, Jorge; Furey, Ambrose; de la Iglesia, Pablo. 2014. "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." Mar. Drugs 12, no. 6: 3706-3732.



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