Improved methodology to survey veterinary antibiotics in environmental samples using µSPEed microextraction followed by ultraperformance liquid chromatography

Abstract A μSPEed microextraction combined with ultra-performance liquid chromatography (UHPLC) with UV detection was developed for analysing six veterinary antibiotics (tetracycline, chlortetracycline, oxytetracycline, doxycycline, sulfamethoxazole, and trimethoprim) in environmental samples. To op...

Full description

Saved in:
Bibliographic Details
Main Authors: Joanna Antos, Laura García-Cansino, María Ángeles García, Dobrochna Ginter-Kramarczyk, María Luisa Marina, Joanna Zembrzuska, José S. Câmara, Jorge A. M. Pereira
Format: Article
Language:English
Published: Nature Portfolio 2025-03-01
Series:Communications Chemistry
Online Access:https://doi.org/10.1038/s42004-025-01454-w
Tags: Add Tag
No Tags, Be the first to tag this record!
_version_ 1849761720269012992
author Joanna Antos
Laura García-Cansino
María Ángeles García
Dobrochna Ginter-Kramarczyk
María Luisa Marina
Joanna Zembrzuska
José S. Câmara
Jorge A. M. Pereira
author_facet Joanna Antos
Laura García-Cansino
María Ángeles García
Dobrochna Ginter-Kramarczyk
María Luisa Marina
Joanna Zembrzuska
José S. Câmara
Jorge A. M. Pereira
author_sort Joanna Antos
collection DOAJ
description Abstract A μSPEed microextraction combined with ultra-performance liquid chromatography (UHPLC) with UV detection was developed for analysing six veterinary antibiotics (tetracycline, chlortetracycline, oxytetracycline, doxycycline, sulfamethoxazole, and trimethoprim) in environmental samples. To optimise extraction, 12 sorbent cartridges, sample loading cycles, volumes, and pH were assayed. The PS/DVB-RP cartridge, three 250 μL sample loading cycles, and two 50-µL elutions with acidified methanol yielded maximum efficiency. The method was validated with optimised fast chromatographic separation, showing good linearity (R2 > 0.99), precision (RSD < 20%), and recoveries between 46-86%. Detection and quantification limits ranged from 0.30-1.23 μg L−1 and 0.92-3.73 μg L−1, respectively. The optimised μSPEed/UPLC-PDA efficiently analysed environmental water samples, requiring only 6 min extraction, 6 min analysis, and 500 μL sample, surpassing alternative methods in speed, workloads and reproducibility. The cost-effective, commercially available equipment facilitates accessibility for laboratories and adaptability for analysing selected antibiotics in diverse matrices, including food and environmental samples.
format Article
id doaj-art-d213d533d9e94447bbac353483f8fa21
institution DOAJ
issn 2399-3669
language English
publishDate 2025-03-01
publisher Nature Portfolio
record_format Article
series Communications Chemistry
spelling doaj-art-d213d533d9e94447bbac353483f8fa212025-08-20T03:05:56ZengNature PortfolioCommunications Chemistry2399-36692025-03-01811810.1038/s42004-025-01454-wImproved methodology to survey veterinary antibiotics in environmental samples using µSPEed microextraction followed by ultraperformance liquid chromatographyJoanna Antos0Laura García-Cansino1María Ángeles García2Dobrochna Ginter-Kramarczyk3María Luisa Marina4Joanna Zembrzuska5José S. Câmara6Jorge A. M. Pereira7CQM—Centro de Química da Madeira, Universidade da Madeira, Campus da PenteadaCQM—Centro de Química da Madeira, Universidade da Madeira, Campus da PenteadaUniversidad de Alcalá, Departamento de Química Analítica, Química Física e Ingeniería Química, Ctra. Madrid-Barcelona Km. 33.600Department of Water Supply and Bioeconomy, Faculty of Environmental Engineering and Energy, Poznan University of Technology, Berdychowo 4Universidad de Alcalá, Departamento de Química Analítica, Química Física e Ingeniería Química, Ctra. Madrid-Barcelona Km. 33.600Faculty of Chemical Technology Institute of Chemistry and Technical Electrochemistry, Berdychowo 4CQM—Centro de Química da Madeira, Universidade da Madeira, Campus da PenteadaCQM—Centro de Química da Madeira, Universidade da Madeira, Campus da PenteadaAbstract A μSPEed microextraction combined with ultra-performance liquid chromatography (UHPLC) with UV detection was developed for analysing six veterinary antibiotics (tetracycline, chlortetracycline, oxytetracycline, doxycycline, sulfamethoxazole, and trimethoprim) in environmental samples. To optimise extraction, 12 sorbent cartridges, sample loading cycles, volumes, and pH were assayed. The PS/DVB-RP cartridge, three 250 μL sample loading cycles, and two 50-µL elutions with acidified methanol yielded maximum efficiency. The method was validated with optimised fast chromatographic separation, showing good linearity (R2 > 0.99), precision (RSD < 20%), and recoveries between 46-86%. Detection and quantification limits ranged from 0.30-1.23 μg L−1 and 0.92-3.73 μg L−1, respectively. The optimised μSPEed/UPLC-PDA efficiently analysed environmental water samples, requiring only 6 min extraction, 6 min analysis, and 500 μL sample, surpassing alternative methods in speed, workloads and reproducibility. The cost-effective, commercially available equipment facilitates accessibility for laboratories and adaptability for analysing selected antibiotics in diverse matrices, including food and environmental samples.https://doi.org/10.1038/s42004-025-01454-w
spellingShingle Joanna Antos
Laura García-Cansino
María Ángeles García
Dobrochna Ginter-Kramarczyk
María Luisa Marina
Joanna Zembrzuska
José S. Câmara
Jorge A. M. Pereira
Improved methodology to survey veterinary antibiotics in environmental samples using µSPEed microextraction followed by ultraperformance liquid chromatography
Communications Chemistry
title Improved methodology to survey veterinary antibiotics in environmental samples using µSPEed microextraction followed by ultraperformance liquid chromatography
title_full Improved methodology to survey veterinary antibiotics in environmental samples using µSPEed microextraction followed by ultraperformance liquid chromatography
title_fullStr Improved methodology to survey veterinary antibiotics in environmental samples using µSPEed microextraction followed by ultraperformance liquid chromatography
title_full_unstemmed Improved methodology to survey veterinary antibiotics in environmental samples using µSPEed microextraction followed by ultraperformance liquid chromatography
title_short Improved methodology to survey veterinary antibiotics in environmental samples using µSPEed microextraction followed by ultraperformance liquid chromatography
title_sort improved methodology to survey veterinary antibiotics in environmental samples using µspeed microextraction followed by ultraperformance liquid chromatography
url https://doi.org/10.1038/s42004-025-01454-w
work_keys_str_mv AT joannaantos improvedmethodologytosurveyveterinaryantibioticsinenvironmentalsamplesusingμspeedmicroextractionfollowedbyultraperformanceliquidchromatography
AT lauragarciacansino improvedmethodologytosurveyveterinaryantibioticsinenvironmentalsamplesusingμspeedmicroextractionfollowedbyultraperformanceliquidchromatography
AT mariaangelesgarcia improvedmethodologytosurveyveterinaryantibioticsinenvironmentalsamplesusingμspeedmicroextractionfollowedbyultraperformanceliquidchromatography
AT dobrochnaginterkramarczyk improvedmethodologytosurveyveterinaryantibioticsinenvironmentalsamplesusingμspeedmicroextractionfollowedbyultraperformanceliquidchromatography
AT marialuisamarina improvedmethodologytosurveyveterinaryantibioticsinenvironmentalsamplesusingμspeedmicroextractionfollowedbyultraperformanceliquidchromatography
AT joannazembrzuska improvedmethodologytosurveyveterinaryantibioticsinenvironmentalsamplesusingμspeedmicroextractionfollowedbyultraperformanceliquidchromatography
AT josescamara improvedmethodologytosurveyveterinaryantibioticsinenvironmentalsamplesusingμspeedmicroextractionfollowedbyultraperformanceliquidchromatography
AT jorgeampereira improvedmethodologytosurveyveterinaryantibioticsinenvironmentalsamplesusingμspeedmicroextractionfollowedbyultraperformanceliquidchromatography