Determination of lipophilic marine toxins in mussels. Quantificationand confirmation criteria using high resolution mass spectrometry

tA multitoxin method has been developed for quantification and confirmation of lipophilic marine biotox-ins in mussels by liquid chromatography coupled to high resolution mass spectrometry (HRMS), using anOrbitrap-Exactive HCD mass spectrometer. Okadaic acid (OA), yessotoxin, azaspiracid-1, gymnodim...

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Detalles Bibliográficos
Autores: Domènech, Albert, Cortés Francisco, Nuria, Palacios Bonilla, Òscar, Franco, José M., Riobó, Pilar, Llerena, José J., Vichi, S. (Stefania), Caixach Gamisans, Josep
Tipo de recurso: artículo
Estado:Versión aceptada para publicación
Fecha de publicación:2013
País:España
Institución:Universidad de Barcelona
Repositorio:Dipòsit Digital de la UB
OAI Identifier:oai:diposit.ub.edu:2445/132799
Acceso en línea:https://hdl.handle.net/2445/132799
Access Level:acceso abierto
Palabra clave:Zoologia
Química analítica
Musclos
Cromatografia
Toxines
Zoology
Analytical chemistry
Mussels
Chromatography
Toxins
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spelling Determination of lipophilic marine toxins in mussels. Quantificationand confirmation criteria using high resolution mass spectrometryDomènech, AlbertCortés Francisco, NuriaPalacios Bonilla, ÒscarFranco, José M.Riobó, PilarLlerena, José J.Vichi, S. (Stefania)Caixach Gamisans, JosepZoologiaQuímica analíticaMusclosCromatografiaToxinesZoologyAnalytical chemistryMusselsChromatographyToxinstA multitoxin method has been developed for quantification and confirmation of lipophilic marine biotox-ins in mussels by liquid chromatography coupled to high resolution mass spectrometry (HRMS), using anOrbitrap-Exactive HCD mass spectrometer. Okadaic acid (OA), yessotoxin, azaspiracid-1, gymnodimine,13-desmethyl spirolide C, pectenotoxin-2 and Brevetoxin B were analyzed as representative compoundsof each lipophilic toxin group. HRMS identification and confirmation criteria were established. Fragmentand isotope ions and ion ratios were studied and evaluated for confirmation purpose. In depth character-ization of full scan and fragmentation spectrum of the main toxins were carried out. Accuracy (truenessand precision), linearity, calibration curve check, limit of quantification (LOQ) and specificity were theparameters established for the method validation. The validation was performed at 0.5 times the currentEuropean Union permitted levels. The method performed very well for the parameters investigated. Thetrueness, expressed as recovery, ranged from 80% to 94%, the precision, expressed as intralaboratoryreproducibility, ranged from 5% to 22% and the LOQs range from 0.9 to 4.8 pg on column. Uncertaintyof the method was also estimated for OA, using a certified reference material. A top-down approachconsidering two main contributions: those arising from the trueness studies and those coming from theprecision's determination, was used. An overall expanded uncertainty of 38% was obtained.Elsevier B.V.2013info:eu-repo/semantics/articleinfo:eu-repo/semantics/acceptedVersionapplication/pdfhttps://hdl.handle.net/2445/132799Articles publicats en revistes (Nutrició, Ciències de l'Alimentació i Gastronomia)reponame:Dipòsit Digital de la UBinstname:Universidad de BarcelonaInglésVersió postprint del document publicat a: https://doi.org/10.1016/j.chroma.2013.12.071Journal of Chromatography A, 2014, vol. 1328, p. 16-25https://doi.org/10.1016/j.chroma.2013.12.071(c) Elsevier B.V., 2014info:eu-repo/semantics/openAccessoai:diposit.ub.edu:2445/1327992026-05-27T06:46:51Z
dc.title.none.fl_str_mv Determination of lipophilic marine toxins in mussels. Quantificationand confirmation criteria using high resolution mass spectrometry
title Determination of lipophilic marine toxins in mussels. Quantificationand confirmation criteria using high resolution mass spectrometry
spellingShingle Determination of lipophilic marine toxins in mussels. Quantificationand confirmation criteria using high resolution mass spectrometry
Domènech, Albert
Zoologia
Química analítica
Musclos
Cromatografia
Toxines
Zoology
Analytical chemistry
Mussels
Chromatography
Toxins
title_short Determination of lipophilic marine toxins in mussels. Quantificationand confirmation criteria using high resolution mass spectrometry
title_full Determination of lipophilic marine toxins in mussels. Quantificationand confirmation criteria using high resolution mass spectrometry
title_fullStr Determination of lipophilic marine toxins in mussels. Quantificationand confirmation criteria using high resolution mass spectrometry
title_full_unstemmed Determination of lipophilic marine toxins in mussels. Quantificationand confirmation criteria using high resolution mass spectrometry
title_sort Determination of lipophilic marine toxins in mussels. Quantificationand confirmation criteria using high resolution mass spectrometry
dc.creator.none.fl_str_mv Domènech, Albert
Cortés Francisco, Nuria
Palacios Bonilla, Òscar
Franco, José M.
Riobó, Pilar
Llerena, José J.
Vichi, S. (Stefania)
Caixach Gamisans, Josep
author Domènech, Albert
author_facet Domènech, Albert
Cortés Francisco, Nuria
Palacios Bonilla, Òscar
Franco, José M.
Riobó, Pilar
Llerena, José J.
Vichi, S. (Stefania)
Caixach Gamisans, Josep
author_role author
author2 Cortés Francisco, Nuria
Palacios Bonilla, Òscar
Franco, José M.
Riobó, Pilar
Llerena, José J.
Vichi, S. (Stefania)
Caixach Gamisans, Josep
author2_role author
author
author
author
author
author
author
dc.subject.none.fl_str_mv Zoologia
Química analítica
Musclos
Cromatografia
Toxines
Zoology
Analytical chemistry
Mussels
Chromatography
Toxins
topic Zoologia
Química analítica
Musclos
Cromatografia
Toxines
Zoology
Analytical chemistry
Mussels
Chromatography
Toxins
description tA multitoxin method has been developed for quantification and confirmation of lipophilic marine biotox-ins in mussels by liquid chromatography coupled to high resolution mass spectrometry (HRMS), using anOrbitrap-Exactive HCD mass spectrometer. Okadaic acid (OA), yessotoxin, azaspiracid-1, gymnodimine,13-desmethyl spirolide C, pectenotoxin-2 and Brevetoxin B were analyzed as representative compoundsof each lipophilic toxin group. HRMS identification and confirmation criteria were established. Fragmentand isotope ions and ion ratios were studied and evaluated for confirmation purpose. In depth character-ization of full scan and fragmentation spectrum of the main toxins were carried out. Accuracy (truenessand precision), linearity, calibration curve check, limit of quantification (LOQ) and specificity were theparameters established for the method validation. The validation was performed at 0.5 times the currentEuropean Union permitted levels. The method performed very well for the parameters investigated. Thetrueness, expressed as recovery, ranged from 80% to 94%, the precision, expressed as intralaboratoryreproducibility, ranged from 5% to 22% and the LOQs range from 0.9 to 4.8 pg on column. Uncertaintyof the method was also estimated for OA, using a certified reference material. A top-down approachconsidering two main contributions: those arising from the trueness studies and those coming from theprecision's determination, was used. An overall expanded uncertainty of 38% was obtained.
publishDate 2013
dc.date.none.fl_str_mv 2013
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/acceptedVersion
format article
status_str acceptedVersion
dc.identifier.none.fl_str_mv https://hdl.handle.net/2445/132799
url https://hdl.handle.net/2445/132799
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv Versió postprint del document publicat a: https://doi.org/10.1016/j.chroma.2013.12.071
Journal of Chromatography A, 2014, vol. 1328, p. 16-25
https://doi.org/10.1016/j.chroma.2013.12.071
dc.rights.none.fl_str_mv (c) Elsevier B.V., 2014
info:eu-repo/semantics/openAccess
rights_invalid_str_mv (c) Elsevier B.V., 2014
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Elsevier B.V.
publisher.none.fl_str_mv Elsevier B.V.
dc.source.none.fl_str_mv Articles publicats en revistes (Nutrició, Ciències de l'Alimentació i Gastronomia)
reponame:Dipòsit Digital de la UB
instname:Universidad de Barcelona
instname_str Universidad de Barcelona
reponame_str Dipòsit Digital de la UB
collection Dipòsit Digital de la UB
repository.name.fl_str_mv
repository.mail.fl_str_mv
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score 15,300719

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