Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry

In this work, a method is proposed for the simultaneous analysis of several pristine fullerenes (C60, C70, C76, C78, and C84) and three C60-fullerene derivatives (N-methyl fulleropyrrolidine, [6,6]-Phenyl C61 butyric acid methyl ester and [6,6]-Phenyl C61 butyric acid buthyl ester) in environmental...

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Authors: Astefanei, Alina, Núñez Burcio, Oscar, Galcerán Huguet, M. Teresa
Format: article
Status:Versión aceptada para publicación
Publication Date:2014
Country:España
Institution:Universidad de Barcelona
Repository:Dipòsit Digital de la UB
OAI Identifier:oai:diposit.ub.edu:2445/99043
Online Access:https://hdl.handle.net/2445/99043
Access Level:Open access
Keyword:Ful·lerens
Espectrometria de masses
Cromatografia de líquids d'alta resolució
Mostreig mediambiental
Fullerenes
Mass spectrometry
High performance liquid chromatography
Environmental sampling
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spelling Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometryAstefanei, AlinaNúñez Burcio, OscarGalcerán Huguet, M. TeresaFul·lerensEspectrometria de massesCromatografia de líquids d'alta resolucióMostreig mediambientalFullerenesMass spectrometryHigh performance liquid chromatographyEnvironmental samplingIn this work, a method is proposed for the simultaneous analysis of several pristine fullerenes (C60, C70, C76, C78, and C84) and three C60-fullerene derivatives (N-methyl fulleropyrrolidine, [6,6]-Phenyl C61 butyric acid methyl ester and [6,6]-Phenyl C61 butyric acid buthyl ester) in environmental samples. The method involves the use of ultrahigh performance liquid chromatography coupled to atmospheric pressure photoionization mass spectrometry (UHPLC-APPI-MS) and allowed the chromatographic separation in less than 4.5 minutes. The product ions from tandem mass spectrometry studies of fullerene derivatives, were characterized and the most abundant one (m/z 720), corresponding to [C60]-¿, was selected for quantitation. Selected reaction monitoring (SRM at 0.7 m/z FWHM) by acquiring two transitions using both isotopic cluster ions [M]-¿ and [M+1]-¿ as precursor ions was proposed for quantitation and confirmation purposes. For pristine fullerenes, highly-selective selected ion monitoring (H-SIM) acquisition mode by monitoring the isotopic cluster ions [M]-¿ and [M+1]-¿ was used. Pressurized solvent extraction conditions were optimized in order to improve recoveries of the studied fullerene compounds from sediment samples. Values up to 87-92% for C60-fullerene derivatives and lower but still acceptable, 70-80%, for pristine fullerenes were obtained. Method limits of quantitation (MLOQs) ranging from 1.5 pg L-1to 5.5 ng L-1 in water samples and from 0.1 ng Kg-1 to 523 ng Kg-1 in sediments were obtained with good precision (relative standard deviations always lower than 13%). The applicability of the developed method was evaluated by analyzing several environmental samples such as sediments and pond water and the detected levels for C60-fullerene derivatives were of 0.1-2.7 ng Kg-1and 1.5-8.5 pg L-1, respectively. C60 and C70 were the only pristine fullerenes detected in the analyzed samples (0.1-7.2 ng Kg-1 in sediments and 9-330 pg L-1 in water pond samples).Elsevier B.V.2014info:eu-repo/semantics/articleinfo:eu-repo/semantics/acceptedVersionapplication/pdfhttps://hdl.handle.net/2445/99043Articles 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.2014.08.089Journal of Chromatography A, 2014, vol. 1365, p. 61-71http://dx.doi.org/10.1016/j.chroma.2014.08.089(c) Elsevier B.V., 2014info:eu-repo/semantics/openAccessoai:diposit.ub.edu:2445/990432026-05-27T06:46:51Z
dc.title.none.fl_str_mv Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry
title Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry
spellingShingle Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry
Astefanei, Alina
Ful·lerens
Espectrometria de masses
Cromatografia de líquids d'alta resolució
Mostreig mediambiental
Fullerenes
Mass spectrometry
High performance liquid chromatography
Environmental sampling
title_short Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry
title_full Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry
title_fullStr Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry
title_full_unstemmed Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry
title_sort Analysis of C60-fullerene fullerene derivatives and pristine fullerenes in environmental samples by ultrahigh performance liquid chromatography-atmospheric pressure photoionization-mass spectrometry
dc.creator.none.fl_str_mv Astefanei, Alina
Núñez Burcio, Oscar
Galcerán Huguet, M. Teresa
author Astefanei, Alina
author_facet Astefanei, Alina
Núñez Burcio, Oscar
Galcerán Huguet, M. Teresa
author_role author
author2 Núñez Burcio, Oscar
Galcerán Huguet, M. Teresa
author2_role author
author
dc.subject.none.fl_str_mv Ful·lerens
Espectrometria de masses
Cromatografia de líquids d'alta resolució
Mostreig mediambiental
Fullerenes
Mass spectrometry
High performance liquid chromatography
Environmental sampling
topic Ful·lerens
Espectrometria de masses
Cromatografia de líquids d'alta resolució
Mostreig mediambiental
Fullerenes
Mass spectrometry
High performance liquid chromatography
Environmental sampling
description In this work, a method is proposed for the simultaneous analysis of several pristine fullerenes (C60, C70, C76, C78, and C84) and three C60-fullerene derivatives (N-methyl fulleropyrrolidine, [6,6]-Phenyl C61 butyric acid methyl ester and [6,6]-Phenyl C61 butyric acid buthyl ester) in environmental samples. The method involves the use of ultrahigh performance liquid chromatography coupled to atmospheric pressure photoionization mass spectrometry (UHPLC-APPI-MS) and allowed the chromatographic separation in less than 4.5 minutes. The product ions from tandem mass spectrometry studies of fullerene derivatives, were characterized and the most abundant one (m/z 720), corresponding to [C60]-¿, was selected for quantitation. Selected reaction monitoring (SRM at 0.7 m/z FWHM) by acquiring two transitions using both isotopic cluster ions [M]-¿ and [M+1]-¿ as precursor ions was proposed for quantitation and confirmation purposes. For pristine fullerenes, highly-selective selected ion monitoring (H-SIM) acquisition mode by monitoring the isotopic cluster ions [M]-¿ and [M+1]-¿ was used. Pressurized solvent extraction conditions were optimized in order to improve recoveries of the studied fullerene compounds from sediment samples. Values up to 87-92% for C60-fullerene derivatives and lower but still acceptable, 70-80%, for pristine fullerenes were obtained. Method limits of quantitation (MLOQs) ranging from 1.5 pg L-1to 5.5 ng L-1 in water samples and from 0.1 ng Kg-1 to 523 ng Kg-1 in sediments were obtained with good precision (relative standard deviations always lower than 13%). The applicability of the developed method was evaluated by analyzing several environmental samples such as sediments and pond water and the detected levels for C60-fullerene derivatives were of 0.1-2.7 ng Kg-1and 1.5-8.5 pg L-1, respectively. C60 and C70 were the only pristine fullerenes detected in the analyzed samples (0.1-7.2 ng Kg-1 in sediments and 9-330 pg L-1 in water pond samples).
publishDate 2014
dc.date.none.fl_str_mv 2014
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/2445/99043
url https://hdl.handle.net/2445/99043
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.2014.08.089
Journal of Chromatography A, 2014, vol. 1365, p. 61-71
http://dx.doi.org/10.1016/j.chroma.2014.08.089
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 (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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