Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts

This work presents a greener approach for ultrasound-assisted (UA) dispersive liquid-liquid microextraction (DLLME) of carbonyl compounds from coffee samples, before GC–MS determination. This work aims to substitute the solvents used in the traditional DLLME procedures with greener alternatives and...

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Detalhes bibliográficos
Autores: Rangel Silva, Alexandra, Custodio Mendoza, Jorge Antonio, Rodrigo Santos, João, Almeida, Paulo Jorge Silva, Rodrigues, José António Maia, Carro Díaz, Antonia María
Tipo de documento: artigo
Data de publicação:2025
País:España
Recursos:Universidad de Santiago de Compostela (USC)
Repositório:Minerva. Repositorio Institucional de la Universidad de Santiago de Compostela
Idioma:inglês
OAI Identifier:oai:minerva.usc.gal:10347/43302
Acesso em linha:https://hdl.handle.net/10347/43302
Access Level:Acceso aberto
Palavra-chave:Carbonyl compounds
Coffee
Dispersive liquid-liquid microextraction
GC-MS
Low-density extractant solvent
Sample preparation
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spelling Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extractsRangel Silva, AlexandraCustodio Mendoza, Jorge AntonioRodrigo Santos, JoãoAlmeida, Paulo Jorge SilvaRodrigues, José António MaiaCarro Díaz, Antonia MaríaCarbonyl compoundsCoffeeDispersive liquid-liquid microextractionGC-MSLow-density extractant solventSample preparationThis work presents a greener approach for ultrasound-assisted (UA) dispersive liquid-liquid microextraction (DLLME) of carbonyl compounds from coffee samples, before GC–MS determination. This work aims to substitute the solvents used in the traditional DLLME procedures with greener alternatives and to decrease the volume of solvents used. Low-density solvents, 1-octanol and isooctane, were evaluated as the extraction solvent. Optimization of critical experimental parameters was conducted in two stages: an asymmetrical screening design 2331 // 8, followed by a Doehlert experimental design. In the first experimental design 4 parameters were optimized: the volume of aqueous phase volume (1.5 mL), the concentration of the derivatization reagent solution pentafluorophenylhydrazine (1.12 g/L) and the volume and type of extraction solvent (60 µL of isooctane). In the second experimental design, 15 min of derivatization at 50 °C were selected as optimized conditions. The enrichment factor associated with the DLLME procedure enabled the efficient extraction of nine carbonyl compounds (acetaldehyde, acrolein, benzaldehyde, diacetyl, formaldehyde, furfural, glyoxal, malondialdehyde, and methylglyoxal) from coffee samples. The method demonstrated strong analytical performance, with figures of merit including r2 ≥ 0.9990, limits of detection between 289 and 436 µg/L, intraday, and interday precisions < 9.5 %. Recovery values for all nine carbonyl compounds ranged from 90.0 to 110.0 %. The greenness of the developed methodology was assessed using the AGREEprep tool, yielding a score of 0.59. Acetaldehyde, benzaldehyde and furfural were quantified in most coffee samples analyzed, with no significant differences observed in carbonyl compounds composition.ElsevierUniversidade de Santiago de Compostela. Instituto de Materiais (iMATUS)20252025-03-2920252025-03-29journal articlehttp://purl.org/coar/resource_type/c_6501VoRhttp://purl.org/coar/version/c_970fb48d4fbd8a85info:eu-repo/semantics/articleapplication/pdfhttps://hdl.handle.net/10347/43302reponame:Minerva. Repositorio Institucional de la Universidad de Santiago de Compostelainstname:Universidad de Santiago de Compostela (USC)Inglésengopen accesshttp://purl.org/coar/access_right/c_abf2© 2025 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).http://creativecommons.org/licenses/by/4.0/info:eu-repo/semantics/openAccessoai:minerva.usc.gal:10347/433022026-06-15T12:47:27Z
dc.title.none.fl_str_mv Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts
title Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts
spellingShingle Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts
Rangel Silva, Alexandra
Carbonyl compounds
Coffee
Dispersive liquid-liquid microextraction
GC-MS
Low-density extractant solvent
Sample preparation
title_short Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts
title_full Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts
title_fullStr Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts
title_full_unstemmed Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts
title_sort Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts
dc.creator.none.fl_str_mv Rangel Silva, Alexandra
Custodio Mendoza, Jorge Antonio
Rodrigo Santos, João
Almeida, Paulo Jorge Silva
Rodrigues, José António Maia
Carro Díaz, Antonia María
author Rangel Silva, Alexandra
author_facet Rangel Silva, Alexandra
Custodio Mendoza, Jorge Antonio
Rodrigo Santos, João
Almeida, Paulo Jorge Silva
Rodrigues, José António Maia
Carro Díaz, Antonia María
author_role author
author2 Custodio Mendoza, Jorge Antonio
Rodrigo Santos, João
Almeida, Paulo Jorge Silva
Rodrigues, José António Maia
Carro Díaz, Antonia María
author2_role author
author
author
author
author
dc.contributor.none.fl_str_mv Universidade de Santiago de Compostela. Instituto de Materiais (iMATUS)

dc.subject.none.fl_str_mv Carbonyl compounds
Coffee
Dispersive liquid-liquid microextraction
GC-MS
Low-density extractant solvent
Sample preparation
topic Carbonyl compounds
Coffee
Dispersive liquid-liquid microextraction
GC-MS
Low-density extractant solvent
Sample preparation
description This work presents a greener approach for ultrasound-assisted (UA) dispersive liquid-liquid microextraction (DLLME) of carbonyl compounds from coffee samples, before GC–MS determination. This work aims to substitute the solvents used in the traditional DLLME procedures with greener alternatives and to decrease the volume of solvents used. Low-density solvents, 1-octanol and isooctane, were evaluated as the extraction solvent. Optimization of critical experimental parameters was conducted in two stages: an asymmetrical screening design 2331 // 8, followed by a Doehlert experimental design. In the first experimental design 4 parameters were optimized: the volume of aqueous phase volume (1.5 mL), the concentration of the derivatization reagent solution pentafluorophenylhydrazine (1.12 g/L) and the volume and type of extraction solvent (60 µL of isooctane). In the second experimental design, 15 min of derivatization at 50 °C were selected as optimized conditions. The enrichment factor associated with the DLLME procedure enabled the efficient extraction of nine carbonyl compounds (acetaldehyde, acrolein, benzaldehyde, diacetyl, formaldehyde, furfural, glyoxal, malondialdehyde, and methylglyoxal) from coffee samples. The method demonstrated strong analytical performance, with figures of merit including r2 ≥ 0.9990, limits of detection between 289 and 436 µg/L, intraday, and interday precisions < 9.5 %. Recovery values for all nine carbonyl compounds ranged from 90.0 to 110.0 %. The greenness of the developed methodology was assessed using the AGREEprep tool, yielding a score of 0.59. Acetaldehyde, benzaldehyde and furfural were quantified in most coffee samples analyzed, with no significant differences observed in carbonyl compounds composition.
publishDate 2025
dc.date.none.fl_str_mv 2025
2025-03-29
2025
2025-03-29
dc.type.none.fl_str_mv journal article
http://purl.org/coar/resource_type/c_6501
VoR
http://purl.org/coar/version/c_970fb48d4fbd8a85
dc.type.openaire.fl_str_mv info:eu-repo/semantics/article
format article
dc.identifier.none.fl_str_mv https://hdl.handle.net/10347/43302
url https://hdl.handle.net/10347/43302
dc.language.none.fl_str_mv Inglés
eng
language_invalid_str_mv Inglés
language eng
dc.rights.none.fl_str_mv open access
http://purl.org/coar/access_right/c_abf2
http://creativecommons.org/licenses/by/4.0/
dc.rights.openaire.fl_str_mv info:eu-repo/semantics/openAccess
rights_invalid_str_mv open access
http://purl.org/coar/access_right/c_abf2
http://creativecommons.org/licenses/by/4.0/
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
dc.source.none.fl_str_mv reponame:Minerva. Repositorio Institucional de la Universidad de Santiago de Compostela
instname:Universidad de Santiago de Compostela (USC)
instname_str Universidad de Santiago de Compostela (USC)
reponame_str Minerva. Repositorio Institucional de la Universidad de Santiago de Compostela
collection Minerva. Repositorio Institucional de la Universidad de Santiago de Compostela
repository.name.fl_str_mv
repository.mail.fl_str_mv
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