Evaluation of Three Sample Preparation Methods for LC-HRMS Suspect Screening of Contaminants of Emerging Concern in Effluent Wastewater

Suspect screening is a valuable tool for studying the pollution footprint of environmental samples, but the sample preparation (SP) method significantly affects the results. In this study, three SP methods─lyophilization, direct injection, and online solid-phase extraction (SPE)─were evaluated for s...

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Autores: Orlando-Véliz, Dana, Bonansea, Rocío Inés, García-Vara, Manuel, Nikolopoulou, Varvara, López de Alda, Miren
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2025
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/410615
Acceso en línea:http://hdl.handle.net/10261/410615
https://api.elsevier.com/content/abstract/scopus_id/105023835527
Access Level:acceso abierto
Palabra clave:Pollution footprint
Suspect screening
http://metadata.un.org/sdg/13
http://metadata.un.org/sdg/12
http://metadata.un.org/sdg/6
http://metadata.un.org/sdg/11
http://metadata.un.org/sdg/3
http://metadata.un.org/sdg/9
Ensure healthy lives and promote well-being for all at all ages
Ensure availability and sustainable management of water and sanitation for all
Build resilient infrastructure, promote inclusive and sustainable industrialization and foster innovation
Make cities and human settlements inclusive, safe, resilient and sustainable
Ensure sustainable consumption and production patterns
Take urgent action to combat climate change and its impacts
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spelling Evaluation of Three Sample Preparation Methods for LC-HRMS Suspect Screening of Contaminants of Emerging Concern in Effluent WastewaterOrlando-Véliz, DanaBonansea, Rocío InésGarcía-Vara, ManuelNikolopoulou, VarvaraLópez de Alda, MirenPollution footprintSuspect screeninghttp://metadata.un.org/sdg/13http://metadata.un.org/sdg/12http://metadata.un.org/sdg/6http://metadata.un.org/sdg/11http://metadata.un.org/sdg/3http://metadata.un.org/sdg/9Ensure healthy lives and promote well-being for all at all agesEnsure availability and sustainable management of water and sanitation for allBuild resilient infrastructure, promote inclusive and sustainable industrialization and foster innovationMake cities and human settlements inclusive, safe, resilient and sustainableEnsure sustainable consumption and production patternsTake urgent action to combat climate change and its impactsSuspect screening is a valuable tool for studying the pollution footprint of environmental samples, but the sample preparation (SP) method significantly affects the results. In this study, three SP methods─lyophilization, direct injection, and online solid-phase extraction (SPE)─were evaluated for suspect screening of contaminants of emerging concern (CECs) in effluent wastewater using liquid chromatography-high resolution mass spectrometry (LC-HRMS). LC-HRMS was performed with a Q-ToF mass analyzer in both positive and negative electrospray ionization modes, and pollutants were identified using the NORMAN SusDat database. A total of 119 CECs were identified with high confidence (all above level 2a). Of these, 115 were detected using lyophilization, 37 with direct injection, and 49 with online SPE. Principal component analysis revealed distinct patterns for each SP method. In all cases, the pollution profile was dominated by pharmaceuticals, followed by industrial chemicals. Articaine, a local anesthetic previously unreported in the aquatic environment, was the most abundant compound found. Industrial chemicals included phthalates, flame retardants, benzotriazoles, and perfluoroalkyl substances, among others. The remaining identified CECs were personal care products, pesticides, and drugs of abuse. Compound prioritization, based on abundance, persistence, mobility, bioaccumulation potential, and toxicity, identified the antibiotics clindamycin and tiamulin, the analgesic flufenamic acid, the musk fragrance metabolite galaxolidone, and the antidepressant venlafaxine metabolite, O-desmethyl venlafaxine, as top priority. These results highlight the importance of applying an appropriate SP method to obtain a comprehensive CEC footprint in suspect screening analysis and demonstrate the suitability of lyophilization for wastewater characterization.This work was supported by the European Commission (Project PROMISCES, number 101036449) and by the Government of Catalonia (2021 SGR 00753). RIB acknowledges her fellowship from the Technical Support Personnel Subprogram (PTA2019-017397-I/AEI/10.13039/501100011033). The authors thank Begoña Martínez and Josep Pascual from the Consorci Besòs Tordera for the provision of the water samples. Biotage is acknowledged for the gift of on-line SPE columns.Peer reviewedAmerican Chemical Society0000-0001-7980-21420000-0002-9347-2765Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]202520252025info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501Publisher's versioninfo:eu-repo/semantics/publishedVersionhttp://hdl.handle.net/10261/410615https://api.elsevier.com/content/abstract/scopus_id/105023835527reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Inglés#PLACEHOLDER_PARENT_METADATA_VALUE#info:eu-repo/grantAgreement/EC/H2020/101036449Analytical chemistryhttps://doi.org/10.1021/acs.analchem.5c01659Síinfo:eu-repo/semantics/openAccessoai:digital.csic.es:10261/4106152026-05-22T06:33:51Z
dc.title.none.fl_str_mv Evaluation of Three Sample Preparation Methods for LC-HRMS Suspect Screening of Contaminants of Emerging Concern in Effluent Wastewater
title Evaluation of Three Sample Preparation Methods for LC-HRMS Suspect Screening of Contaminants of Emerging Concern in Effluent Wastewater
spellingShingle Evaluation of Three Sample Preparation Methods for LC-HRMS Suspect Screening of Contaminants of Emerging Concern in Effluent Wastewater
Orlando-Véliz, Dana
Pollution footprint
Suspect screening
http://metadata.un.org/sdg/13
http://metadata.un.org/sdg/12
http://metadata.un.org/sdg/6
http://metadata.un.org/sdg/11
http://metadata.un.org/sdg/3
http://metadata.un.org/sdg/9
Ensure healthy lives and promote well-being for all at all ages
Ensure availability and sustainable management of water and sanitation for all
Build resilient infrastructure, promote inclusive and sustainable industrialization and foster innovation
Make cities and human settlements inclusive, safe, resilient and sustainable
Ensure sustainable consumption and production patterns
Take urgent action to combat climate change and its impacts
title_short Evaluation of Three Sample Preparation Methods for LC-HRMS Suspect Screening of Contaminants of Emerging Concern in Effluent Wastewater
title_full Evaluation of Three Sample Preparation Methods for LC-HRMS Suspect Screening of Contaminants of Emerging Concern in Effluent Wastewater
title_fullStr Evaluation of Three Sample Preparation Methods for LC-HRMS Suspect Screening of Contaminants of Emerging Concern in Effluent Wastewater
title_full_unstemmed Evaluation of Three Sample Preparation Methods for LC-HRMS Suspect Screening of Contaminants of Emerging Concern in Effluent Wastewater
title_sort Evaluation of Three Sample Preparation Methods for LC-HRMS Suspect Screening of Contaminants of Emerging Concern in Effluent Wastewater
dc.creator.none.fl_str_mv Orlando-Véliz, Dana
Bonansea, Rocío Inés
García-Vara, Manuel
Nikolopoulou, Varvara
López de Alda, Miren
author Orlando-Véliz, Dana
author_facet Orlando-Véliz, Dana
Bonansea, Rocío Inés
García-Vara, Manuel
Nikolopoulou, Varvara
López de Alda, Miren
author_role author
author2 Bonansea, Rocío Inés
García-Vara, Manuel
Nikolopoulou, Varvara
López de Alda, Miren
author2_role author
author
author
author
dc.contributor.none.fl_str_mv 0000-0001-7980-2142
0000-0002-9347-2765
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv Pollution footprint
Suspect screening
http://metadata.un.org/sdg/13
http://metadata.un.org/sdg/12
http://metadata.un.org/sdg/6
http://metadata.un.org/sdg/11
http://metadata.un.org/sdg/3
http://metadata.un.org/sdg/9
Ensure healthy lives and promote well-being for all at all ages
Ensure availability and sustainable management of water and sanitation for all
Build resilient infrastructure, promote inclusive and sustainable industrialization and foster innovation
Make cities and human settlements inclusive, safe, resilient and sustainable
Ensure sustainable consumption and production patterns
Take urgent action to combat climate change and its impacts
topic Pollution footprint
Suspect screening
http://metadata.un.org/sdg/13
http://metadata.un.org/sdg/12
http://metadata.un.org/sdg/6
http://metadata.un.org/sdg/11
http://metadata.un.org/sdg/3
http://metadata.un.org/sdg/9
Ensure healthy lives and promote well-being for all at all ages
Ensure availability and sustainable management of water and sanitation for all
Build resilient infrastructure, promote inclusive and sustainable industrialization and foster innovation
Make cities and human settlements inclusive, safe, resilient and sustainable
Ensure sustainable consumption and production patterns
Take urgent action to combat climate change and its impacts
description Suspect screening is a valuable tool for studying the pollution footprint of environmental samples, but the sample preparation (SP) method significantly affects the results. In this study, three SP methods─lyophilization, direct injection, and online solid-phase extraction (SPE)─were evaluated for suspect screening of contaminants of emerging concern (CECs) in effluent wastewater using liquid chromatography-high resolution mass spectrometry (LC-HRMS). LC-HRMS was performed with a Q-ToF mass analyzer in both positive and negative electrospray ionization modes, and pollutants were identified using the NORMAN SusDat database. A total of 119 CECs were identified with high confidence (all above level 2a). Of these, 115 were detected using lyophilization, 37 with direct injection, and 49 with online SPE. Principal component analysis revealed distinct patterns for each SP method. In all cases, the pollution profile was dominated by pharmaceuticals, followed by industrial chemicals. Articaine, a local anesthetic previously unreported in the aquatic environment, was the most abundant compound found. Industrial chemicals included phthalates, flame retardants, benzotriazoles, and perfluoroalkyl substances, among others. The remaining identified CECs were personal care products, pesticides, and drugs of abuse. Compound prioritization, based on abundance, persistence, mobility, bioaccumulation potential, and toxicity, identified the antibiotics clindamycin and tiamulin, the analgesic flufenamic acid, the musk fragrance metabolite galaxolidone, and the antidepressant venlafaxine metabolite, O-desmethyl venlafaxine, as top priority. These results highlight the importance of applying an appropriate SP method to obtain a comprehensive CEC footprint in suspect screening analysis and demonstrate the suitability of lyophilization for wastewater characterization.
publishDate 2025
dc.date.none.fl_str_mv 2025
2025
2025
dc.type.none.fl_str_mv info:eu-repo/semantics/article
http://purl.org/coar/resource_type/c_6501
Publisher's version
info:eu-repo/semantics/publishedVersion
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/10261/410615
https://api.elsevier.com/content/abstract/scopus_id/105023835527
url http://hdl.handle.net/10261/410615
https://api.elsevier.com/content/abstract/scopus_id/105023835527
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv #PLACEHOLDER_PARENT_METADATA_VALUE#
info:eu-repo/grantAgreement/EC/H2020/101036449
Analytical chemistry
https://doi.org/10.1021/acs.analchem.5c01659
Sí
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv American Chemical Society
publisher.none.fl_str_mv American Chemical Society
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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