title: Improved solid-phase extraction procedure in the analysis of paralytic shellfish poisoning toxins by liquid chromatography with fluorescence detection.
abstract: The analysis of shellfish extracts for the determination of paralytic shellfish poisoning (PSP) toxins by liquid chromatography with fluorescence detection repeatedly showed the presence of a compound suspected to interfere with gonyautoxin 4. The first aim of this study was to confirm by liquid chromatography coupled to tandem mass spectrometry that this compound was not gonyautoxin 4. The second part of this work was to improve a nonvolumetric C(18) solid-phase extraction (SPE) procedure to evaluate the removal of the interference associated with the recovery of PSP toxins. The cleanup procedure was modified into a volumetric SPE procedure and proved to efficiently and totally remove the interference while recovering from 78 to 85% of the PSP toxins available as commercial standards (saxitoxin, neosaxitoxin, gonyautoxins 1-4) and considered as major PSP toxins in human intoxication, with 85% recovery for gonyautoxin 4. The efficiency of this cleanup procedure was checked on shellfish extracts containing this interference and originating from France and Turkey.
authors.affiliation: Agence Française de Sécurité Sanitaire des Aliments, Unité Toxines Microbiennes, 10 rue Pierre Curie, 94704 Maisons-Alfort Cedex, France. rbire@afssa.fr
authors.forename: Ronel
authors.initials: R
authors.lastname: Biré
authors.forename: Sophie
authors.initials: S
authors.lastname: Krys
authors.forename: Jean-Marc
authors.initials: JM
authors.lastname: Frémy
authors.forename: Sylviane
authors.initials: S
authors.lastname: Dragacci
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D008387:Marine Toxins / Q000032:analysis* / Q000302:isolation & purification; D013058:Mass Spectrometry; D012530:Saxitoxin / Q000031:analogs & derivatives* / Q000032:analysis / Q000302:isolation & purification; D012758:Shellfish / Q000032:analysis*; D013050:Spectrometry, Fluorescence; D014020:Tissue Extracts / Q000737:chemistry
chemical_list: D008387:Marine Toxins; D014020:Tissue Extracts; D012530:Saxitoxin; C034902:neosaxitoxin; C013007:gonyautoxins