Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radish

Parent tetracyclines and their transformation products can be present in vegetables growth in soils amended with manure, treated sewage sludge, or irrigated with reclaimed urban wastewater. The presence of some tetracycline antibiotics and transformation products is already regulated in foodstuffs o...

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Autores: García-Criado, Noelia, Martín Bueno, Julia, Santos Morcillo, Juan Luis, Aparicio Gómez, Irene, Alonso Álvarez, Esteban
Tipo de documento: artigo
Estado:Versão publicada
Data de publicação:2026
País:España
Recursos:Universidad de Sevilla (US)
Repositório:idUS. Depósito de Investigación de la Universidad de Sevilla
OAI Identifier:oai:dnet:idus________::3e537d942700c0fb382aa7f71f9ae451
Acesso em linha:https://hdl.handle.net/11441/185113
https://doi.org/10.1016/j.microc.2026.117682
Access Level:Acceso aberto
Palavra-chave:μ-MSPD
Online SPE
LC-MS/MS
Epimers
Greenness assessment
ComplexGAPI
AGREEprep
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spelling Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radishGarcía-Criado, NoeliaMartín Bueno, JuliaSantos Morcillo, Juan LuisAparicio Gómez, IreneAlonso Álvarez, Estebanμ-MSPDOnline SPELC-MS/MSEpimersGreenness assessmentComplexGAPIAGREEprepParent tetracyclines and their transformation products can be present in vegetables growth in soils amended with manure, treated sewage sludge, or irrigated with reclaimed urban wastewater. The presence of some tetracycline antibiotics and transformation products is already regulated in foodstuffs of animal origin but not yet in vegetables. In this paper, an analytical method is proposed for the determination of seven parent tetracycline antibiotics and six transformation products. Selected transformation products correspond to epimers and dehydration products, which have been reported to be the most toxic ones. The proposed method is based on miniaturized matrix solid-phase dispersion (μ-MSPD) method combined with online solid-phase extraction–liquid chromatography–tandem mass spectrometry (online SPE–LC–MS/MS) determination. The method has been validated in radish edible parts (leaves and bulb), to be used for food monitoring, and in roots, to be used in pollutant plant uptake and translocation studies. Proposed method provides MQLs lower than 5ngg⁻¹ dw, accuracy in the range 85–100%, and RSD% lower than 5.5%, for most of the compounds and matrices. Application of the method to radish samples revealed the presence of transformation products of tetracycline antibiotics even in samples where their respective parent compound was not detected. Greenness assessment, using ComplexGAPI and AGREEprep Green Analytical Chemistry metrics, revealed the highest greenness degree of the proposed method in comparison to other methods reported in literature for determination of tetracycline antibiotics in vegetables.ElsevierQuímica AnalíticaFQM344: Análisis Químico Industrial y MedioambientalMinisterio de Ciencia e Innovación (MICIN). EspañaMinisterio de Ciencia, Innovación y Universidades (MICIU). España2026info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionapplication/pdfapplication/pdfhttps://hdl.handle.net/11441/185113https://doi.org/10.1016/j.microc.2026.117682reponame:idUS. Depósito de Investigación de la Universidad de Sevillainstname:Universidad de Sevilla (US)InglésMicrochemical Journal, 224, 117682. PID2020-117641RB-I00PRE2021–100799https://www.sciencedirect.com/science/article/pii/S0026265X26008842info:eu-repo/semantics/openAccessoai:dnet:idus________::3e537d942700c0fb382aa7f71f9ae4512026-06-17T12:51:07Z
dc.title.none.fl_str_mv Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radish
title Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radish
spellingShingle Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radish
García-Criado, Noelia
μ-MSPD
Online SPE
LC-MS/MS
Epimers
Greenness assessment
ComplexGAPI
AGREEprep
title_short Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radish
title_full Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radish
title_fullStr Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radish
title_full_unstemmed Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radish
title_sort Micro-matrix solid-phase dispersion method for the multiresidue determination of tetracycline antibiotics and their transformation products in radish
dc.creator.none.fl_str_mv García-Criado, Noelia
Martín Bueno, Julia
Santos Morcillo, Juan Luis
Aparicio Gómez, Irene
Alonso Álvarez, Esteban
author García-Criado, Noelia
author_facet García-Criado, Noelia
Martín Bueno, Julia
Santos Morcillo, Juan Luis
Aparicio Gómez, Irene
Alonso Álvarez, Esteban
author_role author
author2 Martín Bueno, Julia
Santos Morcillo, Juan Luis
Aparicio Gómez, Irene
Alonso Álvarez, Esteban
author2_role author
author
author
author
dc.contributor.none.fl_str_mv Química Analítica
FQM344: Análisis Químico Industrial y Medioambiental
Ministerio de Ciencia e Innovación (MICIN). España
Ministerio de Ciencia, Innovación y Universidades (MICIU). España
dc.subject.none.fl_str_mv μ-MSPD
Online SPE
LC-MS/MS
Epimers
Greenness assessment
ComplexGAPI
AGREEprep
topic μ-MSPD
Online SPE
LC-MS/MS
Epimers
Greenness assessment
ComplexGAPI
AGREEprep
description Parent tetracyclines and their transformation products can be present in vegetables growth in soils amended with manure, treated sewage sludge, or irrigated with reclaimed urban wastewater. The presence of some tetracycline antibiotics and transformation products is already regulated in foodstuffs of animal origin but not yet in vegetables. In this paper, an analytical method is proposed for the determination of seven parent tetracycline antibiotics and six transformation products. Selected transformation products correspond to epimers and dehydration products, which have been reported to be the most toxic ones. The proposed method is based on miniaturized matrix solid-phase dispersion (μ-MSPD) method combined with online solid-phase extraction–liquid chromatography–tandem mass spectrometry (online SPE–LC–MS/MS) determination. The method has been validated in radish edible parts (leaves and bulb), to be used for food monitoring, and in roots, to be used in pollutant plant uptake and translocation studies. Proposed method provides MQLs lower than 5ngg⁻¹ dw, accuracy in the range 85–100%, and RSD% lower than 5.5%, for most of the compounds and matrices. Application of the method to radish samples revealed the presence of transformation products of tetracycline antibiotics even in samples where their respective parent compound was not detected. Greenness assessment, using ComplexGAPI and AGREEprep Green Analytical Chemistry metrics, revealed the highest greenness degree of the proposed method in comparison to other methods reported in literature for determination of tetracycline antibiotics in vegetables.
publishDate 2026
dc.date.none.fl_str_mv 2026
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv https://hdl.handle.net/11441/185113
https://doi.org/10.1016/j.microc.2026.117682
url https://hdl.handle.net/11441/185113
https://doi.org/10.1016/j.microc.2026.117682
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv Microchemical Journal, 224, 117682.
PID2020-117641RB-I00
PRE2021–100799
https://www.sciencedirect.com/science/article/pii/S0026265X26008842
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
application/pdf
dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
dc.source.none.fl_str_mv reponame:idUS. Depósito de Investigación de la Universidad de Sevilla
instname:Universidad de Sevilla (US)
instname_str Universidad de Sevilla (US)
reponame_str idUS. Depósito de Investigación de la Universidad de Sevilla
collection idUS. Depósito de Investigación de la Universidad de Sevilla
repository.name.fl_str_mv
repository.mail.fl_str_mv
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