Congener-specific determination of hydroxylated polychlorinated biphenyls by polar-embedded reversed-phase liquid chromatography-tandem mass spectrometry

This paper reports the development of an LC-ESI-MS method for the sensitive determination of hydroxylated polychlorinated biphenyls (OH-PCBs) in human serum samples. Congener-specific separation was achieved by using a polar-embedded stationary phase, previously optimized for the working group, whic...

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Autores: Quintanilla-López, Jesús Eduardo, Galindo-Iranzo, Plácido, Lebrón-Aguilar, Rosa, Gómara, Belén
Tipo de recurso: artículo
Fecha de publicación:2020
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/217706
Acceso en línea:http://hdl.handle.net/10261/217706
Access Level:acceso abierto
Palabra clave:Hydroxylated polychlorinated biphenyls
Liquid chromatography –mass spectrometry
Polar embedded stationary phases
Matrix effect
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spelling Congener-specific determination of hydroxylated polychlorinated biphenyls by polar-embedded reversed-phase liquid chromatography-tandem mass spectrometryQuintanilla-López, Jesús EduardoGalindo-Iranzo, PlácidoLebrón-Aguilar, RosaGómara, BelénHydroxylated polychlorinated biphenylsLiquid chromatography –mass spectrometryPolar embedded stationary phasesMatrix effectThis paper reports the development of an LC-ESI-MS method for the sensitive determination of hydroxylated polychlorinated biphenyls (OH-PCBs) in human serum samples. Congener-specific separation was achieved by using a polar-embedded stationary phase, previously optimized for the working group, which provided better separation of isobaric compounds than the common octadecylsilane phases. MS fragmentation patterns and energies showed differences among OH-PCB congeners, mainly depending on the position of OH-group and the number of chlorine atoms in the molecule, although the most intense transitions were always those corresponding to the neutral loss of an HCl group from the quasi-molecular ion cluster. The method allowed the determination of OH-PCBs with good linearity (dynamic linear range of four orders of magnitude with R higher than 0.995) and precision (relative standard deviations of absolute areas lower than 10%), and with better sensitivity than other similar methods previously described in the literature. Matrix effect has been evaluated and reduced to less than 10% by the addition of isotopically labeled standards and a 10-fold dilution of the final sample extract. The low iLODs provided by the developed method (from 1.2 to 5.4 fg µL for all the OH-PCBs studied, except 4′-OH[sbnd]CB108, whose iLOD was 61 fg µL) allows dilution without losses of detected peaks. Finally, the applicability of the method has been demonstrated by analyzing human serum samples belonging to an interlaboratory exercise.Authors thank Comunidad of Madrid and European funding from FSE and FEDER program (S2018/BAA-4393–AVANSECAL-II- CM) and the Spanish Ministry of Economy and Competitiveness (projects AGL2012–37201 and AGL2016–80475-R) for the financial support. We are particularly grateful to Laura Herrero and Sagrario Calvarro for their technical aidComunidad de MadridEuropean CommissionMinisterio de Economía y Competitividad (España)Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]2020202020202020info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501http://hdl.handle.net/10261/217706reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Inglés#PLACEHOLDER_PARENT_METADATA_VALUE##PLACEHOLDER_PARENT_METADATA_VALUE#info:eu-repo/grantAgreement/MINECO/Plan Estatal de Investigación Científica y Técnica y de Innovación 2013-2016/AGL2016-80475-RS2018/BAA-4393/AVANSECAL-II-CMhttp://dx.doi.org/10.1016/j.chroma.2020.461353Síinfo:eu-repo/semantics/openAccessoai:digital.csic.es:10261/2177062026-05-22T06:33:51Z
dc.title.none.fl_str_mv Congener-specific determination of hydroxylated polychlorinated biphenyls by polar-embedded reversed-phase liquid chromatography-tandem mass spectrometry
title Congener-specific determination of hydroxylated polychlorinated biphenyls by polar-embedded reversed-phase liquid chromatography-tandem mass spectrometry
spellingShingle Congener-specific determination of hydroxylated polychlorinated biphenyls by polar-embedded reversed-phase liquid chromatography-tandem mass spectrometry
Quintanilla-López, Jesús Eduardo
Hydroxylated polychlorinated biphenyls
Liquid chromatography –mass spectrometry
Polar embedded stationary phases
Matrix effect
title_short Congener-specific determination of hydroxylated polychlorinated biphenyls by polar-embedded reversed-phase liquid chromatography-tandem mass spectrometry
title_full Congener-specific determination of hydroxylated polychlorinated biphenyls by polar-embedded reversed-phase liquid chromatography-tandem mass spectrometry
title_fullStr Congener-specific determination of hydroxylated polychlorinated biphenyls by polar-embedded reversed-phase liquid chromatography-tandem mass spectrometry
title_full_unstemmed Congener-specific determination of hydroxylated polychlorinated biphenyls by polar-embedded reversed-phase liquid chromatography-tandem mass spectrometry
title_sort Congener-specific determination of hydroxylated polychlorinated biphenyls by polar-embedded reversed-phase liquid chromatography-tandem mass spectrometry
dc.creator.none.fl_str_mv Quintanilla-López, Jesús Eduardo
Galindo-Iranzo, Plácido
Lebrón-Aguilar, Rosa
Gómara, Belén
author Quintanilla-López, Jesús Eduardo
author_facet Quintanilla-López, Jesús Eduardo
Galindo-Iranzo, Plácido
Lebrón-Aguilar, Rosa
Gómara, Belén
author_role author
author2 Galindo-Iranzo, Plácido
Lebrón-Aguilar, Rosa
Gómara, Belén
author2_role author
author
author
dc.contributor.none.fl_str_mv Comunidad de Madrid
European Commission
Ministerio de Economía y Competitividad (España)
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv Hydroxylated polychlorinated biphenyls
Liquid chromatography –mass spectrometry
Polar embedded stationary phases
Matrix effect
topic Hydroxylated polychlorinated biphenyls
Liquid chromatography –mass spectrometry
Polar embedded stationary phases
Matrix effect
description This paper reports the development of an LC-ESI-MS method for the sensitive determination of hydroxylated polychlorinated biphenyls (OH-PCBs) in human serum samples. Congener-specific separation was achieved by using a polar-embedded stationary phase, previously optimized for the working group, which provided better separation of isobaric compounds than the common octadecylsilane phases. MS fragmentation patterns and energies showed differences among OH-PCB congeners, mainly depending on the position of OH-group and the number of chlorine atoms in the molecule, although the most intense transitions were always those corresponding to the neutral loss of an HCl group from the quasi-molecular ion cluster. The method allowed the determination of OH-PCBs with good linearity (dynamic linear range of four orders of magnitude with R higher than 0.995) and precision (relative standard deviations of absolute areas lower than 10%), and with better sensitivity than other similar methods previously described in the literature. Matrix effect has been evaluated and reduced to less than 10% by the addition of isotopically labeled standards and a 10-fold dilution of the final sample extract. The low iLODs provided by the developed method (from 1.2 to 5.4 fg µL for all the OH-PCBs studied, except 4′-OH[sbnd]CB108, whose iLOD was 61 fg µL) allows dilution without losses of detected peaks. Finally, the applicability of the method has been demonstrated by analyzing human serum samples belonging to an interlaboratory exercise.
publishDate 2020
dc.date.none.fl_str_mv 2020
2020
2020
2020
dc.type.none.fl_str_mv info:eu-repo/semantics/article
http://purl.org/coar/resource_type/c_6501
format article
dc.identifier.none.fl_str_mv http://hdl.handle.net/10261/217706
url http://hdl.handle.net/10261/217706
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv #PLACEHOLDER_PARENT_METADATA_VALUE#
#PLACEHOLDER_PARENT_METADATA_VALUE#
info:eu-repo/grantAgreement/MINECO/Plan Estatal de Investigación Científica y Técnica y de Innovación 2013-2016/AGL2016-80475-R
S2018/BAA-4393/AVANSECAL-II-CM
http://dx.doi.org/10.1016/j.chroma.2020.461353
Sí
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.source.none.fl_str_mv reponame:DIGITAL.CSIC. Repositorio Institucional del CSIC
instname:Consejo Superior de Investigaciones Científicas (CSIC)
instname_str Consejo Superior de Investigaciones Científicas (CSIC)
reponame_str DIGITAL.CSIC. Repositorio Institucional del CSIC
collection DIGITAL.CSIC. Repositorio Institucional del CSIC
repository.name.fl_str_mv
repository.mail.fl_str_mv
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