Strategies for the multi-residue analysis of 100 pesticides by liquid chromatography-triple quadrupole mass spectrometry

Analytical strategies for screening, quantitation and confirmation of a group of 100 pesticides in fruit and vegetable samples by LC-MS and LC-MS/MS were developed. The pesticides studied belong to different chemical families of herbicides, insecticides and fungicides. A selection of some degradatio...

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Autores: Núñez Burcio, Oscar, Gallart Ayala, Hèctor, Ferrer, Imma, Moyano Morcillo, Encarnación, Galcerán Huguet, M. Teresa
Tipo de recurso: artículo
Estado:Versión aceptada para publicación
Fecha de publicación:2012
País:España
Institución:Universidad de Barcelona
Repositorio:Dipòsit Digital de la UB
OAI Identifier:oai:diposit.ub.edu:2445/98263
Acceso en línea:https://hdl.handle.net/2445/98263
Access Level:acceso abierto
Palabra clave:Plaguicides
Química dels aliments
Cromatografia de líquids
Pesticides
Food composition
Liquid chromatography
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spelling Strategies for the multi-residue analysis of 100 pesticides by liquid chromatography-triple quadrupole mass spectrometryNúñez Burcio, OscarGallart Ayala, HèctorFerrer, ImmaMoyano Morcillo, EncarnaciónGalcerán Huguet, M. TeresaPlaguicidesQuímica dels alimentsCromatografia de líquidsPesticidesFood compositionLiquid chromatographyAnalytical strategies for screening, quantitation and confirmation of a group of 100 pesticides in fruit and vegetable samples by LC-MS and LC-MS/MS were developed. The pesticides studied belong to different chemical families of herbicides, insecticides and fungicides. A selection of some degradation products was also included. Chromatographic separation was performed using a Zorbax Eclipse XDB-C8 column (150 mm × 4.6 mm and 5 µm particle size), and gradient elution with acetonitrile-water (both with 0.1% formic acid) as mobile phase. LC-MS/MS using highly-selective selected reaction monitoring (H-SRM) acquisition mode monitoring two transitions for each compound showed to be the most sensitive methodology. Quantitation was carried out using matrix-matched standard calibration and good linearity of response was demonstrated (r > 0.998). Limits of detection (by acquiring two transitions and with the ion-ratio requirements) ranged between 0.01 and 20 µg/kg were obtained. So, in general, the sensitivity achieved meets the maximum residue levels (MRLs) established by the European Union regulation for food monitoring programs. Pesticide confirmation was carried out following European Union guidelines. In order to prevent false-positives, further confirmatory strategies were proposed. LC-MS in highly-selective selected ion monitoring (H-SIM) mode with accurate mass measurement was used to obtain an orthogonal criterion (exact mass) for confirmation. Accurate mass measurements were always bellow 0.9 mDa for almost all pesticides studied (similar to those described with TOF instruments). A user reversed energy ramp (RER) product ion scan spectra library was generated by means of a data dependent analysis for routine library searching of pesticides. The combination of LC-MS/MS in H-SRM mode and the generation of the RER product ion scan spectra and library search were then used to achieve further confirmation on pesticide analysis. The LC-MS and LC-MS/MS strategies developed were successfully applied for the analysis and confirmation of pesticides in different types of fruit and vegetables samples, and examples of the screening, quantitation and confirmation of pesticides in these samples are shown in this work.Elsevier B.V.2012info:eu-repo/semantics/articleinfo:eu-repo/semantics/acceptedVersionapplication/pdfhttps://hdl.handle.net/2445/98263Articles publicats en revistes (Enginyeria Química i Química Analítica)reponame:Dipòsit Digital de la UBinstname:Universidad de BarcelonaInglésVersió postprint del document publicat a: http://dx.doi.org/10.1016/j.chroma.2012.06.028Journal of Chromatography A, 2012, vol. 1249, p. 164-180http://dx.doi.org/10.1016/j.chroma.2012.06.028(c) Elsevier B.V., 2012info:eu-repo/semantics/openAccessoai:diposit.ub.edu:2445/982632026-05-27T06:46:51Z
dc.title.none.fl_str_mv Strategies for the multi-residue analysis of 100 pesticides by liquid chromatography-triple quadrupole mass spectrometry
title Strategies for the multi-residue analysis of 100 pesticides by liquid chromatography-triple quadrupole mass spectrometry
spellingShingle Strategies for the multi-residue analysis of 100 pesticides by liquid chromatography-triple quadrupole mass spectrometry
Núñez Burcio, Oscar
Plaguicides
Química dels aliments
Cromatografia de líquids
Pesticides
Food composition
Liquid chromatography
title_short Strategies for the multi-residue analysis of 100 pesticides by liquid chromatography-triple quadrupole mass spectrometry
title_full Strategies for the multi-residue analysis of 100 pesticides by liquid chromatography-triple quadrupole mass spectrometry
title_fullStr Strategies for the multi-residue analysis of 100 pesticides by liquid chromatography-triple quadrupole mass spectrometry
title_full_unstemmed Strategies for the multi-residue analysis of 100 pesticides by liquid chromatography-triple quadrupole mass spectrometry
title_sort Strategies for the multi-residue analysis of 100 pesticides by liquid chromatography-triple quadrupole mass spectrometry
dc.creator.none.fl_str_mv Núñez Burcio, Oscar
Gallart Ayala, Hèctor
Ferrer, Imma
Moyano Morcillo, Encarnación
Galcerán Huguet, M. Teresa
author Núñez Burcio, Oscar
author_facet Núñez Burcio, Oscar
Gallart Ayala, Hèctor
Ferrer, Imma
Moyano Morcillo, Encarnación
Galcerán Huguet, M. Teresa
author_role author
author2 Gallart Ayala, Hèctor
Ferrer, Imma
Moyano Morcillo, Encarnación
Galcerán Huguet, M. Teresa
author2_role author
author
author
author
dc.subject.none.fl_str_mv Plaguicides
Química dels aliments
Cromatografia de líquids
Pesticides
Food composition
Liquid chromatography
topic Plaguicides
Química dels aliments
Cromatografia de líquids
Pesticides
Food composition
Liquid chromatography
description Analytical strategies for screening, quantitation and confirmation of a group of 100 pesticides in fruit and vegetable samples by LC-MS and LC-MS/MS were developed. The pesticides studied belong to different chemical families of herbicides, insecticides and fungicides. A selection of some degradation products was also included. Chromatographic separation was performed using a Zorbax Eclipse XDB-C8 column (150 mm × 4.6 mm and 5 µm particle size), and gradient elution with acetonitrile-water (both with 0.1% formic acid) as mobile phase. LC-MS/MS using highly-selective selected reaction monitoring (H-SRM) acquisition mode monitoring two transitions for each compound showed to be the most sensitive methodology. Quantitation was carried out using matrix-matched standard calibration and good linearity of response was demonstrated (r > 0.998). Limits of detection (by acquiring two transitions and with the ion-ratio requirements) ranged between 0.01 and 20 µg/kg were obtained. So, in general, the sensitivity achieved meets the maximum residue levels (MRLs) established by the European Union regulation for food monitoring programs. Pesticide confirmation was carried out following European Union guidelines. In order to prevent false-positives, further confirmatory strategies were proposed. LC-MS in highly-selective selected ion monitoring (H-SIM) mode with accurate mass measurement was used to obtain an orthogonal criterion (exact mass) for confirmation. Accurate mass measurements were always bellow 0.9 mDa for almost all pesticides studied (similar to those described with TOF instruments). A user reversed energy ramp (RER) product ion scan spectra library was generated by means of a data dependent analysis for routine library searching of pesticides. The combination of LC-MS/MS in H-SRM mode and the generation of the RER product ion scan spectra and library search were then used to achieve further confirmation on pesticide analysis. The LC-MS and LC-MS/MS strategies developed were successfully applied for the analysis and confirmation of pesticides in different types of fruit and vegetables samples, and examples of the screening, quantitation and confirmation of pesticides in these samples are shown in this work.
publishDate 2012
dc.date.none.fl_str_mv 2012
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/2445/98263
url https://hdl.handle.net/2445/98263
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv Versió postprint del document publicat a: http://dx.doi.org/10.1016/j.chroma.2012.06.028
Journal of Chromatography A, 2012, vol. 1249, p. 164-180
http://dx.doi.org/10.1016/j.chroma.2012.06.028
dc.rights.none.fl_str_mv (c) Elsevier B.V., 2012
info:eu-repo/semantics/openAccess
rights_invalid_str_mv (c) Elsevier B.V., 2012
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 (Enginyeria Química i Química Analítica)
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 15,301629

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