Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvoluti...

Autores
Junqué, Eva; Fernández, Pilar; Filippi, Iohanna; Grimalt, Joan O.
Año de publicación
2023
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
An analytical method for the simultaneous determination of glyphosate (GLY) and its main derivative, aminomethyl-phosphonic acid (AMPA), in human urine has been developed using gas chromatography coupled to tandem mass spectrometry (MS/MS) operated in multiple reaction monitoring mode (MRM). Sample preparation involved dilution of urine with water and derivatization with a mixture of trifluoroacetic acid anhydride and trifluoroethanol. Derivatization conditions such as reaction time and temperature, derivative stability, injection solvent, MS ionization mode and MS-MS transitions, among others, were studied to obtain the highest method sensitivity. The target compounds were initially quantified by the isotope dilution method using isotopically labelled analogs of GLY and AMPA as internal standards. However, due to spectral overlap between GLY and labelled GLY in the selected quantitative transition, a quantification method based on isotope pattern deconvolution (IPD) has been developed. The instrumental limits of detection were 0.05 ng mL−1 for both compounds, while the method detection limits were 0.39 and 0.25 ng mL−1, for AMPA and GLY, respectively. The mean recoveries from urine and water spiked at different concentrations were 77 and 69% for AMPA and 90 and 102% for GLY, respectively, with mean relative standard deviations of 8–10% (urine samples, n = 12) and 3.6–4% (water samples, n = 6). Once validated, the feasibility of the method was tested by determination of AMPA and GLY in human urine samples from people living close to agricultural areas. The developed method affords the determination of these compounds at trace concentrations in complex matrices such as urine, avoiding elaborate handling and cleanup steps. Isotope pattern deconvolution has proven to be a successful alternative to calibration curve for GLY overriding the method uncertainties associated to spectral overlapping.
Fil: Junqué, Eva. Consejo Superior de Investigaciones Científicas; España
Fil: Fernández, Pilar. Consejo Superior de Investigaciones Científicas; España
Fil: Filippi, Iohanna. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Córdoba. Centro de Investigaciones en Bioquímica Clínica e Inmunología; Argentina
Fil: Grimalt, Joan O.. Consejo Superior de Investigaciones Científicas; España
Materia
BIOMONITORING
GAS CHROMATOGRAPHY
ISOTOPE DILUTION
POLAR PESTICIDES
TANDEM MASS SPECTROMETRY IN NEGATIVE ION CHEMICAL IONIZATION
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc-nd/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/226565
Acceder
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oai_identifier_str oai:ri.conicet.gov.ar:11336/226565
network_acronym_str CONICETDig
repository_id_str 3498
network_name_str CONICET Digital (CONICET)
spelling Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolutionJunqué, EvaFernández, PilarFilippi, IohannaGrimalt, Joan O.BIOMONITORINGGAS CHROMATOGRAPHYISOTOPE DILUTIONPOLAR PESTICIDESTANDEM MASS SPECTROMETRY IN NEGATIVE ION CHEMICAL IONIZATIONhttps://purl.org/becyt/ford/3.3https://purl.org/becyt/ford/3An analytical method for the simultaneous determination of glyphosate (GLY) and its main derivative, aminomethyl-phosphonic acid (AMPA), in human urine has been developed using gas chromatography coupled to tandem mass spectrometry (MS/MS) operated in multiple reaction monitoring mode (MRM). Sample preparation involved dilution of urine with water and derivatization with a mixture of trifluoroacetic acid anhydride and trifluoroethanol. Derivatization conditions such as reaction time and temperature, derivative stability, injection solvent, MS ionization mode and MS-MS transitions, among others, were studied to obtain the highest method sensitivity. The target compounds were initially quantified by the isotope dilution method using isotopically labelled analogs of GLY and AMPA as internal standards. However, due to spectral overlap between GLY and labelled GLY in the selected quantitative transition, a quantification method based on isotope pattern deconvolution (IPD) has been developed. The instrumental limits of detection were 0.05 ng mL−1 for both compounds, while the method detection limits were 0.39 and 0.25 ng mL−1, for AMPA and GLY, respectively. The mean recoveries from urine and water spiked at different concentrations were 77 and 69% for AMPA and 90 and 102% for GLY, respectively, with mean relative standard deviations of 8–10% (urine samples, n = 12) and 3.6–4% (water samples, n = 6). Once validated, the feasibility of the method was tested by determination of AMPA and GLY in human urine samples from people living close to agricultural areas. The developed method affords the determination of these compounds at trace concentrations in complex matrices such as urine, avoiding elaborate handling and cleanup steps. Isotope pattern deconvolution has proven to be a successful alternative to calibration curve for GLY overriding the method uncertainties associated to spectral overlapping.Fil: Junqué, Eva. Consejo Superior de Investigaciones Científicas; EspañaFil: Fernández, Pilar. Consejo Superior de Investigaciones Científicas; EspañaFil: Filippi, Iohanna. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Córdoba. Centro de Investigaciones en Bioquímica Clínica e Inmunología; ArgentinaFil: Grimalt, Joan O.. Consejo Superior de Investigaciones Científicas; EspañaElsevier2023-11info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/226565Junqué, Eva; Fernández, Pilar; Filippi, Iohanna; Grimalt, Joan O.; Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution; Elsevier; Journal of Chromatography Open; 4; 11-2023; 1-112772-3917CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/url/https://linkinghub.elsevier.com/retrieve/pii/S2772391723000117info:eu-repo/semantics/altIdentifier/doi/10.1016/j.jcoa.2023.100087info:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-nd/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-10-15T14:58:32Zoai:ri.conicet.gov.ar:11336/226565instacron:CONICETInstitucionalhttp://ri.conicet.gov.ar/Organismo científico-tecnológicoNo correspondehttp://ri.conicet.gov.ar/oai/requestdasensio@conicet.gov.ar; lcarlino@conicet.gov.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:34982025-10-15 14:58:32.549CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution
title Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution
spellingShingle Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution
Junqué, Eva
BIOMONITORING
GAS CHROMATOGRAPHY
ISOTOPE DILUTION
POLAR PESTICIDES
TANDEM MASS SPECTROMETRY IN NEGATIVE ION CHEMICAL IONIZATION
title_short Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution
title_full Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution
title_fullStr Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution
title_full_unstemmed Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution
title_sort Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution
dc.creator.none.fl_str_mv Junqué, Eva
Fernández, Pilar
Filippi, Iohanna
Grimalt, Joan O.
author Junqué, Eva
author_facet Junqué, Eva
Fernández, Pilar
Filippi, Iohanna
Grimalt, Joan O.
author_role author
author2 Fernández, Pilar
Filippi, Iohanna
Grimalt, Joan O.
author2_role author
author
author
dc.subject.none.fl_str_mv BIOMONITORING
GAS CHROMATOGRAPHY
ISOTOPE DILUTION
POLAR PESTICIDES
TANDEM MASS SPECTROMETRY IN NEGATIVE ION CHEMICAL IONIZATION
topic BIOMONITORING
GAS CHROMATOGRAPHY
ISOTOPE DILUTION
POLAR PESTICIDES
TANDEM MASS SPECTROMETRY IN NEGATIVE ION CHEMICAL IONIZATION
purl_subject.fl_str_mv https://purl.org/becyt/ford/3.3
https://purl.org/becyt/ford/3
dc.description.none.fl_txt_mv An analytical method for the simultaneous determination of glyphosate (GLY) and its main derivative, aminomethyl-phosphonic acid (AMPA), in human urine has been developed using gas chromatography coupled to tandem mass spectrometry (MS/MS) operated in multiple reaction monitoring mode (MRM). Sample preparation involved dilution of urine with water and derivatization with a mixture of trifluoroacetic acid anhydride and trifluoroethanol. Derivatization conditions such as reaction time and temperature, derivative stability, injection solvent, MS ionization mode and MS-MS transitions, among others, were studied to obtain the highest method sensitivity. The target compounds were initially quantified by the isotope dilution method using isotopically labelled analogs of GLY and AMPA as internal standards. However, due to spectral overlap between GLY and labelled GLY in the selected quantitative transition, a quantification method based on isotope pattern deconvolution (IPD) has been developed. The instrumental limits of detection were 0.05 ng mL−1 for both compounds, while the method detection limits were 0.39 and 0.25 ng mL−1, for AMPA and GLY, respectively. The mean recoveries from urine and water spiked at different concentrations were 77 and 69% for AMPA and 90 and 102% for GLY, respectively, with mean relative standard deviations of 8–10% (urine samples, n = 12) and 3.6–4% (water samples, n = 6). Once validated, the feasibility of the method was tested by determination of AMPA and GLY in human urine samples from people living close to agricultural areas. The developed method affords the determination of these compounds at trace concentrations in complex matrices such as urine, avoiding elaborate handling and cleanup steps. Isotope pattern deconvolution has proven to be a successful alternative to calibration curve for GLY overriding the method uncertainties associated to spectral overlapping.
Fil: Junqué, Eva. Consejo Superior de Investigaciones Científicas; España
Fil: Fernández, Pilar. Consejo Superior de Investigaciones Científicas; España
Fil: Filippi, Iohanna. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Córdoba. Centro de Investigaciones en Bioquímica Clínica e Inmunología; Argentina
Fil: Grimalt, Joan O.. Consejo Superior de Investigaciones Científicas; España
description An analytical method for the simultaneous determination of glyphosate (GLY) and its main derivative, aminomethyl-phosphonic acid (AMPA), in human urine has been developed using gas chromatography coupled to tandem mass spectrometry (MS/MS) operated in multiple reaction monitoring mode (MRM). Sample preparation involved dilution of urine with water and derivatization with a mixture of trifluoroacetic acid anhydride and trifluoroethanol. Derivatization conditions such as reaction time and temperature, derivative stability, injection solvent, MS ionization mode and MS-MS transitions, among others, were studied to obtain the highest method sensitivity. The target compounds were initially quantified by the isotope dilution method using isotopically labelled analogs of GLY and AMPA as internal standards. However, due to spectral overlap between GLY and labelled GLY in the selected quantitative transition, a quantification method based on isotope pattern deconvolution (IPD) has been developed. The instrumental limits of detection were 0.05 ng mL−1 for both compounds, while the method detection limits were 0.39 and 0.25 ng mL−1, for AMPA and GLY, respectively. The mean recoveries from urine and water spiked at different concentrations were 77 and 69% for AMPA and 90 and 102% for GLY, respectively, with mean relative standard deviations of 8–10% (urine samples, n = 12) and 3.6–4% (water samples, n = 6). Once validated, the feasibility of the method was tested by determination of AMPA and GLY in human urine samples from people living close to agricultural areas. The developed method affords the determination of these compounds at trace concentrations in complex matrices such as urine, avoiding elaborate handling and cleanup steps. Isotope pattern deconvolution has proven to be a successful alternative to calibration curve for GLY overriding the method uncertainties associated to spectral overlapping.
publishDate 2023
dc.date.none.fl_str_mv 2023-11
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
http://purl.org/coar/resource_type/c_6501
info:ar-repo/semantics/articulo
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/11336/226565
Junqué, Eva; Fernández, Pilar; Filippi, Iohanna; Grimalt, Joan O.; Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution; Elsevier; Journal of Chromatography Open; 4; 11-2023; 1-11
2772-3917
CONICET Digital
CONICET
url http://hdl.handle.net/11336/226565
identifier_str_mv Junqué, Eva; Fernández, Pilar; Filippi, Iohanna; Grimalt, Joan O.; Determination of glyphosate and its derivative, aminomethylphosphonic acid, in human urine by gas chromatography coupled to tandem mass spectrometry and isotope pattern deconvolution; Elsevier; Journal of Chromatography Open; 4; 11-2023; 1-11
2772-3917
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/url/https://linkinghub.elsevier.com/retrieve/pii/S2772391723000117
info:eu-repo/semantics/altIdentifier/doi/10.1016/j.jcoa.2023.100087
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc-nd/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc-nd/2.5/ar/
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:CONICET Digital (CONICET)
instname:Consejo Nacional de Investigaciones Científicas y Técnicas
reponame_str CONICET Digital (CONICET)
collection CONICET Digital (CONICET)
instname_str Consejo Nacional de Investigaciones Científicas y Técnicas
repository.name.fl_str_mv CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicas
repository.mail.fl_str_mv dasensio@conicet.gov.ar; lcarlino@conicet.gov.ar
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score 12.891075

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