LC-HRMS and GC-MS profiling of urine free cortisol, cortisone, 6Β-, and 18-Hydroxycortisol for the evaluation of glucocorticoid and mineralocorticoid disorders

Introduction: Urine free cortisol measurements are routinely performed to evaluate hypercortisolism. Despite their analytical inaccuracy, immunoassay-based methods are frequently used. Advances in liquid chromatography-high-resolution mass spectrometry (LC-HRMS) facilitate the incorporation of power...

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Autores: Casals Mercadal, Gregori, Ballesteros Vizoso, María Antonieta, Zamora Trillo, Angielys, Martínez Martín, Irene, Fernández Varo, Guillermo, Mora Porta, Mireia, Hanzu, Felicia A., Morales Ruiz, Manuel
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2024
País:España
Institución:Varias* (Consorci de Biblioteques Universitáries de Catalunya, Centre de Serveis Científics i Acadèmics de Catalunya)
Repositorio:Recercat. Dipósit de la Recerca de Catalunya
OAI Identifier:oai:recercat.cat:2445/222548
Acceso en línea:https://hdl.handle.net/2445/222548
Access Level:acceso abierto
Palabra clave:Cromatografia de líquids
Cortisona
Síndrome de Cushing
Liquid chromatography
Cortisone
Cushing's syndrome
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spelling LC-HRMS and GC-MS profiling of urine free cortisol, cortisone, 6Β-, and 18-Hydroxycortisol for the evaluation of glucocorticoid and mineralocorticoid disordersCasals Mercadal, GregoriBallesteros Vizoso, María AntonietaZamora Trillo, AngielysMartínez Martín, IreneFernández Varo, GuillermoMora Porta, MireiaHanzu, Felicia A.Morales Ruiz, ManuelCromatografia de líquidsCortisonaSíndrome de CushingLiquid chromatographyCortisoneCushing's syndromeIntroduction: Urine free cortisol measurements are routinely performed to evaluate hypercortisolism. Despite their analytical inaccuracy, immunoassay-based methods are frequently used. Advances in liquid chromatography-high-resolution mass spectrometry (LC-HRMS) facilitate the incorporation of powerful diagnostic tools into clinical laboratories. In addition to its high analytical specificity and simultaneous analysis of different metabolites, accurate mass measurement allows for untargeted compound identification, which may help to identify clinically relevant metabolites or drugs. Methods: The present study aimed to validate a simple routine LC-HRMS method to quantify cortisol, cortisone, 6β-hydroxycortisol, and 18-hydroxycortisol simultaneously in human urine. Additionally, the study also validated a GC-MS method for the same steroids, evaluated their cross-reactivity with commercial cortisol immunoassays, and quantified the 24 h urine excretion in patients under clinical suspicion or follow-up for hypercortisolism. Results: The LC-HRMS method involved liquid-liquid extraction using dichloromethane, micro-LC for chromatographic separation and detection using the accurate masses of the steroids, and simultaneous high-resolution full scan acquisition. The method presented acceptable linearity, precision, and accuracy. Significant interference from 6β-hydroxycortisol and cortisone was demonstrated in the cortisol immunoassays, which impacted their reliability in the follow-up of patients with hypercortisolism and significant changes in these cortisol metabolites (i.e., due to drug-induced changes in CYP3A4 activity). Conclusion: A rapid and accurate routine LC-HRMS method was validated, which is useful for the evaluation of hypercortisolism and other disorders of glucocorticoid and mineralocorticoid metabolism.MDPI2025202520242025info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersion16 p.application/pdfhttps://hdl.handle.net/2445/222548Articles publicats en revistes (Infermeria Fonamental i Clínica)reponame:Recercat. Dipósit de la Recerca de Catalunyainstname:Varias* (Consorci de Biblioteques Universitáries de Catalunya, Centre de Serveis Científics i Acadèmics de Catalunya)InglésReproducció del document publicat a: https://doi.org/10.3390/biom14050558Biomolecules, 2024, vol. 14, num.5https://doi.org/10.3390/biom14050558cc-by (c) Casals, G. et al., 2024http://creativecommons.org/licenses/by/4.0/info:eu-repo/semantics/openAccessoai:recercat.cat:2445/2225482026-05-29T05:05:01Z
dc.title.none.fl_str_mv LC-HRMS and GC-MS profiling of urine free cortisol, cortisone, 6Β-, and 18-Hydroxycortisol for the evaluation of glucocorticoid and mineralocorticoid disorders
title LC-HRMS and GC-MS profiling of urine free cortisol, cortisone, 6Β-, and 18-Hydroxycortisol for the evaluation of glucocorticoid and mineralocorticoid disorders
spellingShingle LC-HRMS and GC-MS profiling of urine free cortisol, cortisone, 6Β-, and 18-Hydroxycortisol for the evaluation of glucocorticoid and mineralocorticoid disorders
Casals Mercadal, Gregori
Cromatografia de líquids
Cortisona
Síndrome de Cushing
Liquid chromatography
Cortisone
Cushing's syndrome
title_short LC-HRMS and GC-MS profiling of urine free cortisol, cortisone, 6Β-, and 18-Hydroxycortisol for the evaluation of glucocorticoid and mineralocorticoid disorders
title_full LC-HRMS and GC-MS profiling of urine free cortisol, cortisone, 6Β-, and 18-Hydroxycortisol for the evaluation of glucocorticoid and mineralocorticoid disorders
title_fullStr LC-HRMS and GC-MS profiling of urine free cortisol, cortisone, 6Β-, and 18-Hydroxycortisol for the evaluation of glucocorticoid and mineralocorticoid disorders
title_full_unstemmed LC-HRMS and GC-MS profiling of urine free cortisol, cortisone, 6Β-, and 18-Hydroxycortisol for the evaluation of glucocorticoid and mineralocorticoid disorders
title_sort LC-HRMS and GC-MS profiling of urine free cortisol, cortisone, 6Β-, and 18-Hydroxycortisol for the evaluation of glucocorticoid and mineralocorticoid disorders
dc.creator.none.fl_str_mv Casals Mercadal, Gregori
Ballesteros Vizoso, María Antonieta
Zamora Trillo, Angielys
Martínez Martín, Irene
Fernández Varo, Guillermo
Mora Porta, Mireia
Hanzu, Felicia A.
Morales Ruiz, Manuel
author Casals Mercadal, Gregori
author_facet Casals Mercadal, Gregori
Ballesteros Vizoso, María Antonieta
Zamora Trillo, Angielys
Martínez Martín, Irene
Fernández Varo, Guillermo
Mora Porta, Mireia
Hanzu, Felicia A.
Morales Ruiz, Manuel
author_role author
author2 Ballesteros Vizoso, María Antonieta
Zamora Trillo, Angielys
Martínez Martín, Irene
Fernández Varo, Guillermo
Mora Porta, Mireia
Hanzu, Felicia A.
Morales Ruiz, Manuel
author2_role author
author
author
author
author
author
author
dc.subject.none.fl_str_mv Cromatografia de líquids
Cortisona
Síndrome de Cushing
Liquid chromatography
Cortisone
Cushing's syndrome
topic Cromatografia de líquids
Cortisona
Síndrome de Cushing
Liquid chromatography
Cortisone
Cushing's syndrome
description Introduction: Urine free cortisol measurements are routinely performed to evaluate hypercortisolism. Despite their analytical inaccuracy, immunoassay-based methods are frequently used. Advances in liquid chromatography-high-resolution mass spectrometry (LC-HRMS) facilitate the incorporation of powerful diagnostic tools into clinical laboratories. In addition to its high analytical specificity and simultaneous analysis of different metabolites, accurate mass measurement allows for untargeted compound identification, which may help to identify clinically relevant metabolites or drugs. Methods: The present study aimed to validate a simple routine LC-HRMS method to quantify cortisol, cortisone, 6β-hydroxycortisol, and 18-hydroxycortisol simultaneously in human urine. Additionally, the study also validated a GC-MS method for the same steroids, evaluated their cross-reactivity with commercial cortisol immunoassays, and quantified the 24 h urine excretion in patients under clinical suspicion or follow-up for hypercortisolism. Results: The LC-HRMS method involved liquid-liquid extraction using dichloromethane, micro-LC for chromatographic separation and detection using the accurate masses of the steroids, and simultaneous high-resolution full scan acquisition. The method presented acceptable linearity, precision, and accuracy. Significant interference from 6β-hydroxycortisol and cortisone was demonstrated in the cortisol immunoassays, which impacted their reliability in the follow-up of patients with hypercortisolism and significant changes in these cortisol metabolites (i.e., due to drug-induced changes in CYP3A4 activity). Conclusion: A rapid and accurate routine LC-HRMS method was validated, which is useful for the evaluation of hypercortisolism and other disorders of glucocorticoid and mineralocorticoid metabolism.
publishDate 2024
dc.date.none.fl_str_mv 2024
2025
2025
2025
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/2445/222548
url https://hdl.handle.net/2445/222548
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv Reproducció del document publicat a: https://doi.org/10.3390/biom14050558
Biomolecules, 2024, vol. 14, num.5
https://doi.org/10.3390/biom14050558
dc.rights.none.fl_str_mv cc-by (c) Casals, G. et al., 2024
http://creativecommons.org/licenses/by/4.0/
info:eu-repo/semantics/openAccess
rights_invalid_str_mv cc-by (c) Casals, G. et al., 2024
http://creativecommons.org/licenses/by/4.0/
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv 16 p.
application/pdf
dc.publisher.none.fl_str_mv MDPI
publisher.none.fl_str_mv MDPI
dc.source.none.fl_str_mv Articles publicats en revistes (Infermeria Fonamental i Clínica)
reponame:Recercat. Dipósit de la Recerca de Catalunya
instname:Varias* (Consorci de Biblioteques Universitáries de Catalunya, Centre de Serveis Científics i Acadèmics de Catalunya)
instname_str Varias* (Consorci de Biblioteques Universitáries de Catalunya, Centre de Serveis Científics i Acadèmics de Catalunya)
reponame_str Recercat. Dipósit de la Recerca de Catalunya
collection Recercat. Dipósit de la Recerca de Catalunya
repository.name.fl_str_mv
repository.mail.fl_str_mv
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