Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluids

This review examines recent advancements in high-throughput sample treatment for mass spectrometric analysis of organic xenobiotics in human biofluids. The first section explores emerging techniques using solid, liquid and polymeric sorbents, emphasizing configurations that enhance batch processing...

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Main Authors: Esther González-Infante, Anne San Román, Juan F. Ayala-Cabrera, Nestor Etxebarria, Belén González-Gaya, Naroa Lopez-Herguedas, Mikel Musatadi, Maitane Olivares, Ailette Prieto, Olatz Zuloaga
Format: Article
Language:English
Published: Elsevier 2025-05-01
Series:Advances in Sample Preparation
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Online Access:http://www.sciencedirect.com/science/article/pii/S2772582025000361
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author Esther González-Infante
Anne San Román
Juan F. Ayala-Cabrera
Nestor Etxebarria
Belén González-Gaya
Naroa Lopez-Herguedas
Mikel Musatadi
Maitane Olivares
Ailette Prieto
Olatz Zuloaga
author_facet Esther González-Infante
Anne San Román
Juan F. Ayala-Cabrera
Nestor Etxebarria
Belén González-Gaya
Naroa Lopez-Herguedas
Mikel Musatadi
Maitane Olivares
Ailette Prieto
Olatz Zuloaga
author_sort Esther González-Infante
collection DOAJ
description This review examines recent advancements in high-throughput sample treatment for mass spectrometric analysis of organic xenobiotics in human biofluids. The first section explores emerging techniques using solid, liquid and polymeric sorbents, emphasizing configurations that enhance batch processing and environmental sustainability. Innovations in solid-phase (micro)extraction and liquid-liquid (micro)extraction are discussed, along with advancements in sorbent materials. Additionally, centrifugal-assisted sample treatment is highlighted as a complementary technique that streamlines key steps, including protein precipitation. Special attention is also given to direct infusion and ambient ionization-based mass spectrometry, which significantly reduce analysis time by eliminating chromatographic separation. Automation, crucial for handling large sample volumes in clinical and biomonitoring studies, is also emphasized. The second section reviews recent applications of high-throughput techniques for detecting organic xenobiotics in human biofluids via mass spectrometry. While the primary focus is on urine and blood/plasma/serum, other biofluids such as breast milk, oral fluid, semen and cerebrospinal fluid are also considered. Most studies aim to increase sample throughput via automation, batch processing, or direct analysis, while miniaturization and novel sorbents remain less explored. Research remains largely centered on legal and illegal drug analysis, with fewer studies addressing exogenous xenobiotics such as pesticides, industrial chemicals, or endocrine-disrupting chemicals. Further efforts are needed to develop methods capable of detecting a broad spectrum of compounds within a single workflow. Finally, establishing standardized metrics to quantitatively assess throughput beyond traditional figures of merit is essential for defining high-throughput sample preparation in a meaningful and universally accepted manner.
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spelling doaj-art-35df6ff3350c4e5787788cf8e2de18eb2025-08-20T02:15:58ZengElsevierAdvances in Sample Preparation2772-58202025-05-011410018310.1016/j.sampre.2025.100183Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluidsEsther González-Infante0Anne San Román1Juan F. Ayala-Cabrera2Nestor Etxebarria3Belén González-Gaya4Naroa Lopez-Herguedas5Mikel Musatadi6Maitane Olivares7Ailette Prieto8Olatz Zuloaga9Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena s/n, 48940, Leioa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (Plentzia Marine Station, PiE-UPV/EHU), University of the Basque Country (UPV/EHU), Areatza Hiribidea, 47, 48620 Plentzia, Bizkaia, Basque Country, Spain; Corresponding authors.Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena s/n, 48940, Leioa, Basque Country, Spain; Institute of Health Research Biodonostia, Paseo Dr. Begiristain, s/n, 20014 Donostia Gipuzkoa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (Plentzia Marine Station, PiE-UPV/EHU), University of the Basque Country (UPV/EHU), Areatza Hiribidea, 47, 48620 Plentzia, Bizkaia, Basque Country, Spain; Corresponding authors.Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena s/n, 48940, Leioa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (Plentzia Marine Station, PiE-UPV/EHU), University of the Basque Country (UPV/EHU), Areatza Hiribidea, 47, 48620 Plentzia, Bizkaia, Basque Country, SpainDepartment of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena s/n, 48940, Leioa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (Plentzia Marine Station, PiE-UPV/EHU), University of the Basque Country (UPV/EHU), Areatza Hiribidea, 47, 48620 Plentzia, Bizkaia, Basque Country, SpainDepartment of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena s/n, 48940, Leioa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (Plentzia Marine Station, PiE-UPV/EHU), University of the Basque Country (UPV/EHU), Areatza Hiribidea, 47, 48620 Plentzia, Bizkaia, Basque Country, Spain; IKERBASQUE, Basque Foundation for Science, Plaza Euskadi 5, 48009 Bilbao, SpainDepartment of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena s/n, 48940, Leioa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (Plentzia Marine Station, PiE-UPV/EHU), University of the Basque Country (UPV/EHU), Areatza Hiribidea, 47, 48620 Plentzia, Bizkaia, Basque Country, Spain; Department of Cell Toxicology, Helmholtz Centre for Environmental Research - UFZ, Permoserstr. 15, 04318 Leipzig, GermanyDepartment of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena s/n, 48940, Leioa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (Plentzia Marine Station, PiE-UPV/EHU), University of the Basque Country (UPV/EHU), Areatza Hiribidea, 47, 48620 Plentzia, Bizkaia, Basque Country, SpainDepartment of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena s/n, 48940, Leioa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (Plentzia Marine Station, PiE-UPV/EHU), University of the Basque Country (UPV/EHU), Areatza Hiribidea, 47, 48620 Plentzia, Bizkaia, Basque Country, SpainDepartment of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena s/n, 48940, Leioa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (Plentzia Marine Station, PiE-UPV/EHU), University of the Basque Country (UPV/EHU), Areatza Hiribidea, 47, 48620 Plentzia, Bizkaia, Basque Country, SpainDepartment of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Barrio Sarriena s/n, 48940, Leioa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (Plentzia Marine Station, PiE-UPV/EHU), University of the Basque Country (UPV/EHU), Areatza Hiribidea, 47, 48620 Plentzia, Bizkaia, Basque Country, SpainThis review examines recent advancements in high-throughput sample treatment for mass spectrometric analysis of organic xenobiotics in human biofluids. The first section explores emerging techniques using solid, liquid and polymeric sorbents, emphasizing configurations that enhance batch processing and environmental sustainability. Innovations in solid-phase (micro)extraction and liquid-liquid (micro)extraction are discussed, along with advancements in sorbent materials. Additionally, centrifugal-assisted sample treatment is highlighted as a complementary technique that streamlines key steps, including protein precipitation. Special attention is also given to direct infusion and ambient ionization-based mass spectrometry, which significantly reduce analysis time by eliminating chromatographic separation. Automation, crucial for handling large sample volumes in clinical and biomonitoring studies, is also emphasized. The second section reviews recent applications of high-throughput techniques for detecting organic xenobiotics in human biofluids via mass spectrometry. While the primary focus is on urine and blood/plasma/serum, other biofluids such as breast milk, oral fluid, semen and cerebrospinal fluid are also considered. Most studies aim to increase sample throughput via automation, batch processing, or direct analysis, while miniaturization and novel sorbents remain less explored. Research remains largely centered on legal and illegal drug analysis, with fewer studies addressing exogenous xenobiotics such as pesticides, industrial chemicals, or endocrine-disrupting chemicals. Further efforts are needed to develop methods capable of detecting a broad spectrum of compounds within a single workflow. Finally, establishing standardized metrics to quantitatively assess throughput beyond traditional figures of merit is essential for defining high-throughput sample preparation in a meaningful and universally accepted manner.http://www.sciencedirect.com/science/article/pii/S2772582025000361High-throughputSample treatmentMass spectrometryHuman biofluidsOrganic xenobiotics
spellingShingle Esther González-Infante
Anne San Román
Juan F. Ayala-Cabrera
Nestor Etxebarria
Belén González-Gaya
Naroa Lopez-Herguedas
Mikel Musatadi
Maitane Olivares
Ailette Prieto
Olatz Zuloaga
Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluids
Advances in Sample Preparation
High-throughput
Sample treatment
Mass spectrometry
Human biofluids
Organic xenobiotics
title Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluids
title_full Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluids
title_fullStr Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluids
title_full_unstemmed Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluids
title_short Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluids
title_sort mass spectrometry based high throughput sample treatment methods for analysis of xenobiotics in human biofluids
topic High-throughput
Sample treatment
Mass spectrometry
Human biofluids
Organic xenobiotics
url http://www.sciencedirect.com/science/article/pii/S2772582025000361
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