{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,4,8]],"date-time":"2026-04-08T01:15:32Z","timestamp":1775610932478,"version":"3.50.1"},"reference-count":43,"publisher":"MDPI AG","issue":"22","license":[{"start":{"date-parts":[[2024,11,20]],"date-time":"2024-11-20T00:00:00Z","timestamp":1732060800000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"DOI":"10.13039\/501100004837","name":"Ministerio de Ciencia e Innovaci\u00f3n-Agencia Estatal de Investigaci\u00f3n","doi-asserted-by":"publisher","award":["PID2020-117641RB-I00"],"award-info":[{"award-number":["PID2020-117641RB-I00"]}],"id":[{"id":"10.13039\/501100004837","id-type":"DOI","asserted-by":"publisher"}]},{"DOI":"10.13039\/501100004837","name":"Ministerio de Ciencia e Innovaci\u00f3n-Agencia Estatal de Investigaci\u00f3n","doi-asserted-by":"publisher","award":["VI PPIT-US 2021 II.2A"],"award-info":[{"award-number":["VI PPIT-US 2021 II.2A"]}],"id":[{"id":"10.13039\/501100004837","id-type":"DOI","asserted-by":"publisher"}]},{"DOI":"10.13039\/501100004837","name":"Ministerio de Ciencia e Innovaci\u00f3n-Agencia Estatal de Investigaci\u00f3n","doi-asserted-by":"publisher","award":["VIIPPIT-2024-EBRV"],"award-info":[{"award-number":["VIIPPIT-2024-EBRV"]}],"id":[{"id":"10.13039\/501100004837","id-type":"DOI","asserted-by":"publisher"}]},{"DOI":"10.13039\/100009042","name":"University of Seville","doi-asserted-by":"publisher","award":["PID2020-117641RB-I00"],"award-info":[{"award-number":["PID2020-117641RB-I00"]}],"id":[{"id":"10.13039\/100009042","id-type":"DOI","asserted-by":"publisher"}]},{"DOI":"10.13039\/100009042","name":"University of Seville","doi-asserted-by":"publisher","award":["VI PPIT-US 2021 II.2A"],"award-info":[{"award-number":["VI PPIT-US 2021 II.2A"]}],"id":[{"id":"10.13039\/100009042","id-type":"DOI","asserted-by":"publisher"}]},{"DOI":"10.13039\/100009042","name":"University of Seville","doi-asserted-by":"publisher","award":["VIIPPIT-2024-EBRV"],"award-info":[{"award-number":["VIIPPIT-2024-EBRV"]}],"id":[{"id":"10.13039\/100009042","id-type":"DOI","asserted-by":"publisher"}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Molecules"],"abstract":"<jats:p>The presence of antibiotics in seafood for human consumption may pose a risk for consumers. Furthermore, some marine organisms, such as mussels, can result in appropriate bioindicators of marine contamination. In this work, a multiresidue analytical methodology suitable for the determination of antibiotics and metabolites in mussels is proposed. The target compounds include three sulphonamides and trimethoprim (TMP) and six of their main metabolites. Sample treatment involves extraction and clean-up in a single step using matrix solid-phase dispersion with acetonitrile. Analytical determination was carried out by liquid chromatography\u2013tandem mass spectrometry. Good linearity (R2 &gt; 0.99), accuracy (from 80.8 to 118%), and limits of quantification (lower than 5 ng g\u22121 (dry matter, dm)) were obtained for all selected compounds. The method was applied to the determination of antibiotics in mussel samples from an exposure assay with contaminated seawater with TMP and sulfamethoxazole (SMX). Both antibiotics were detected in the analysed samples with concentrations up to 77.5 ng g\u22121 dm. TMP was bioconcentrated to a higher extent than SMX, attributable to its higher hydrophobicity. None of the metabolites were detected. These results demonstrate that Mytilus galloprovincialis is a suitable bioindicator to assess marine pollution.<\/jats:p>","DOI":"10.3390\/molecules29225478","type":"journal-article","created":{"date-parts":[[2024,11,20]],"date-time":"2024-11-20T09:14:38Z","timestamp":1732094078000},"page":"5478","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Matrix Solid-Phase Dispersion Procedure for Determination of Antibiotics and Metabolites in Mussels: Application in Exposure Bioassays"],"prefix":"10.3390","volume":"29","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-7966-830X","authenticated-orcid":false,"given":"Carmen","family":"Mej\u00edas","sequence":"first","affiliation":[{"name":"Departamento de Qu\u00edmica Anal\u00edtica, Escuela Polit\u00e9cnica Superior, Universidad de Sevilla, C\/Virgen de \u00c1frica, 7, E-41011 Seville, Spain"}]},{"given":"Tain\u00e1 G.","family":"Fonseca","sequence":"additional","affiliation":[{"name":"Centre for Marine and Environmental Research\u2014CIMA\/ARNET\u2014Infrastructure Network in Aquatic Research, University of Algarve, Campus de Gambelas, 8000-139 Faro, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7775-3367","authenticated-orcid":false,"given":"Noelia","family":"Garc\u00eda-Criado","sequence":"additional","affiliation":[{"name":"Departamento de Qu\u00edmica Anal\u00edtica, Escuela Polit\u00e9cnica Superior, Universidad de Sevilla, C\/Virgen de \u00c1frica, 7, E-41011 Seville, Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3621-1291","authenticated-orcid":false,"given":"Julia","family":"Mart\u00edn","sequence":"additional","affiliation":[{"name":"Departamento de Qu\u00edmica Anal\u00edtica, Escuela Polit\u00e9cnica Superior, Universidad de Sevilla, C\/Virgen de \u00c1frica, 7, E-41011 Seville, Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9704-1316","authenticated-orcid":false,"given":"Juan Luis","family":"Santos","sequence":"additional","affiliation":[{"name":"Departamento de Qu\u00edmica Anal\u00edtica, Escuela Polit\u00e9cnica Superior, Universidad de Sevilla, C\/Virgen de \u00c1frica, 7, E-41011 Seville, Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5468-9021","authenticated-orcid":false,"given":"Irene","family":"Aparicio","sequence":"additional","affiliation":[{"name":"Departamento de Qu\u00edmica Anal\u00edtica, Escuela Polit\u00e9cnica Superior, Universidad de Sevilla, C\/Virgen de \u00c1frica, 7, E-41011 Seville, Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1647-9226","authenticated-orcid":false,"given":"Esteban","family":"Alonso","sequence":"additional","affiliation":[{"name":"Departamento de Qu\u00edmica Anal\u00edtica, Escuela Polit\u00e9cnica Superior, Universidad de Sevilla, C\/Virgen de \u00c1frica, 7, E-41011 Seville, Spain"}]}],"member":"1968","published-online":{"date-parts":[[2024,11,20]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","unstructured":"European Centre for Disease Prevention and Control (ECDC), European Food Safety Authority (EFSA), and European Medicines Agency (EMA) (2024). Antimicrobial consumption and resistance in bacteria from humans and food-producing animals. Fourth joint inter-agency report on integrated analysis of antimicrobial agent consumption and occurrence of antimicrobial resistance in bacteria from humans and food-producing animals in the EU\/EEA. JIACRA IV 2019\u20132021. EFSA J., 22, e8589.","DOI":"10.2903\/j.efsa.2024.p220201"},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"391","DOI":"10.1016\/j.marpolbul.2013.12.045","article-title":"Emerging organic contaminants in coastal waters: Anthropogenic impact, environmental release and ecological risk","volume":"85","author":"Jiang","year":"2014","journal-title":"Mar. Pollut. Bull."},{"key":"ref_3","first-page":"329","article-title":"Sources and occurrence of pharmaceutical residues in offshore seawater","volume":"Volume 1","year":"2021","journal-title":"Pharmaceuticals in Marine and Coastal Environments. Occurrence, Effects and Challenges in a Changing World"},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"1097","DOI":"10.1016\/j.scitotenv.2015.09.145","article-title":"Occurrence and spatial distribution of 158 pharmaceuticals, drugs of abuse and related metabolites in offshore seawater","volume":"541","author":"Alygizakis","year":"2016","journal-title":"Sci. Total Environ."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"62","DOI":"10.1016\/j.marpolbul.2015.03.008","article-title":"Contamination of the southern Baltic Sea waters by the residues of selected pharmaceuticals: Method development and field studies","volume":"94","author":"Borecka","year":"2015","journal-title":"Mar. Pollut. Bull."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"5795","DOI":"10.1021\/es0629965","article-title":"Distributions of pharmaceuticals in an urban estuary during both dry and wet-weather conditions","volume":"41","author":"Benotti","year":"2007","journal-title":"Environ. Sci. Technol."},{"key":"ref_7","unstructured":"World Health Organization (2024, October 05). Fact Sheet: Antibiotic Resistance. Available online: https:\/\/www.who.int\/news-room\/fact-sheets\/detail\/antibiotic-resistance."},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"317","DOI":"10.1016\/j.scitotenv.2013.12.123","article-title":"A year-long study of the spatial occurrence and relative distribution of pharmaceutical residues in sewage effluent, receiving marine waters and marine bivalves","volume":"476\u2013477","author":"McEneff","year":"2014","journal-title":"Sci. Total Environ."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"3","DOI":"10.1016\/j.fct.2016.11.031","article-title":"Multi-residue for the determination of antibiotics and some of their metabolites in seafood","volume":"104","year":"2017","journal-title":"Food Chem. Toxicol."},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"763","DOI":"10.1016\/j.envpol.2019.02.060","article-title":"Occurrence and level of emerging organic contaminant in fish and mollusk from Klang River estuary, Malaysia and assessment on human health risk","volume":"248","author":"Omar","year":"2019","journal-title":"Environ. Pollut."},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"122155","DOI":"10.1016\/j.envpol.2023.122155","article-title":"Indigenous food sources as vectors of Escherichia coli and antibiotic resistance","volume":"334","author":"Kurenbach","year":"2023","journal-title":"Environ. Pollut."},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"174268","DOI":"10.1016\/j.scitotenv.2024.174268","article-title":"Microplastic ingestion in mussels from the East Mediterranean Sea: Exploring its impacts in nature and controlled conditions","volume":"946","author":"Digka","year":"2024","journal-title":"Sci. Total Environ."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"600","DOI":"10.1016\/j.envpol.2018.11.038","article-title":"An assessment of the ability to ingest and excrete microplastics by filter-feeders: A case study with the Mediterranean mussel","volume":"245","author":"Martins","year":"2019","journal-title":"Environ. Pollut."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"104314","DOI":"10.1016\/j.etap.2023.104314","article-title":"Comparative subcellular responses to pharmaceutical exposures in the mussel Mytilus galloprovincialis: An in vitro study","volume":"104","author":"Cruz","year":"2023","journal-title":"Environ. Toxicol. Pharmacol."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"174","DOI":"10.1016\/j.talanta.2014.12.035","article-title":"Multi-residue method for the analysis of pharmaceuticals and some of their metabolites in bivalves","volume":"136","author":"Huerta","year":"2015","journal-title":"Talanta"},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"9509","DOI":"10.1007\/s00216-013-7371-6","article-title":"The determination of pharmaceutical residues in cooked and uncooked marine bivalves using pressurised liquid extraction, solid-phase extraction and liquid chromatography-tandem mass spectrometry","volume":"405","author":"McEneff","year":"2013","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"156","DOI":"10.1016\/j.aca.2010.07.026","article-title":"Application of enzymatic probe sonication extraction for the determination of selected veterinary antibiotics and their main metabolites in fish and mussel samples","volume":"675","year":"2010","journal-title":"Anal. Chim. Acta"},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"1146","DOI":"10.1016\/j.jpba.2010.12.002","article-title":"Enzymatic-microwave assisted extraction and high-performance liquid chromatography-mass spectrometry for the determination of selected veterinary antibiotics in fish and mussel samples","volume":"54","year":"2011","journal-title":"J. Pharm. Biomed. Anal."},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"151","DOI":"10.1016\/j.jbbm.2006.06.005","article-title":"Matrix solid phase dispersion (MSPD)","volume":"70","author":"Barker","year":"2007","journal-title":"J. Biochem. Biophys. Methods"},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"3957","DOI":"10.1039\/D4AY00738G","article-title":"Optimization of a modified Captiva EMR-lipid method based on micro-matrix solid-phase dispersion coupled with gas chromatography-mass spectrometry for the determination of nine bisphenols in mussel samples","volume":"16","author":"Carro","year":"2024","journal-title":"Anal. Methods"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"100714","DOI":"10.1016\/j.focha.2024.100714","article-title":"Optimization of an analytical method based on miniaturized matrix solid-phase dispersion combined with gas chromatography-mass spectrometry for the determination of bisphenols in mussel samples","volume":"4","author":"Carro","year":"2024","journal-title":"Food Chem."},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"537","DOI":"10.1080\/19440049.2024.2334300","article-title":"Optimization of a fast and sensitive method based on matrix solid-phase dispersion-LC-MS\/MS for simultaneous determination of phthalates and bisphenols in mussel simples","volume":"41","author":"Castellani","year":"2024","journal-title":"Food Addit. Contam. Part A"},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"51","DOI":"10.1186\/s40543-021-00303-4","article-title":"Fast determination of phthalates in mussel samples by micro-matrix solid-phase dispersion (micro-MSPD) coupled with GC\u2013MS\/MS","volume":"12","author":"Carro","year":"2021","journal-title":"J. Anal. Sci. Technol."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"603","DOI":"10.1134\/S1061934821050099","article-title":"Development and Optimization of a Method for Organochlorine Pesticides Determination in Mussels Based on Miniaturized Matrix Solid-Phase Dispersion Combined with Gas Chromatography\u2013Tandem Mass Spectrometry","volume":"76","author":"Carro","year":"2021","journal-title":"J. Anal. Chem."},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"57","DOI":"10.1016\/j.chroma.2016.06.070","article-title":"Matrix solid-phase dispersion combined to liquid chromatography\u2013tandem mass spectrometry for the determination of paraben preservatives in mollusks","volume":"1459","author":"Rodil","year":"2016","journal-title":"J. Chromatogr. A"},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1016\/j.ancr.2016.11.003","article-title":"Optimization of a method based on micro-matrix solid-phase dispersion (micro-MSPD) for the determination of PCBs in mussel samples","volume":"11","author":"Carro","year":"2017","journal-title":"Anal. Chem. Res."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"391","DOI":"10.1016\/j.foodchem.2014.09.153","article-title":"Development of a Matrix Solid Phase Dispersion methodology for the determination of triazine herbicides in mussels","volume":"173","year":"2015","journal-title":"Food Chem."},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"11","DOI":"10.1080\/03067319.2012.702277","article-title":"Optimization of matrix solid-phase dispersion conditions for UV filters determination in biota samples","volume":"93","author":"Negreira","year":"2013","journal-title":"Int. J. Environ. Anal. Chem."},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"509","DOI":"10.1007\/s00216-011-5302-y","article-title":"Determination of perfluorinated compounds in mollusks by matrix solid-phase dispersion and liquid chromatography\u2013tandem mass spectrometry","volume":"402","author":"Quintana","year":"2012","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"120470","DOI":"10.1016\/j.talanta.2019.120470","article-title":"Determination of 18 organophosphorus flame retardants\/plasticizers in mussel samples by matrix solid-phase dispersion combined to liquid chromatography-tandem mass spectrometry","volume":"208","author":"Castro","year":"2020","journal-title":"Talanta"},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"85","DOI":"10.1016\/j.chroma.2013.05.064","article-title":"Matrix solid-phase dispersion combined with gas chromatography\u2013mass spectrometry for the determination of fifteen halogenated flame retardants in mollusks","volume":"1300","author":"Quintana","year":"2013","journal-title":"J. Chromatogr. A"},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"100255","DOI":"10.1016\/j.talo.2023.100255","article-title":"Rapid fabrication of magnetic covalent organic frameworks for the effective extraction and determination of sulfonamides in shrimp samples","volume":"8","author":"Sun","year":"2023","journal-title":"Talanta Open"},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"104718","DOI":"10.1016\/j.jfca.2022.104718","article-title":"Development and evaluation of a semi-automatic single-step clean-up apparatus for rapid analysis of 18 antibiotics in fish samples","volume":"113","author":"Mu","year":"2022","journal-title":"J. Food Comp. Anal."},{"key":"ref_34","doi-asserted-by":"crossref","unstructured":"Bitas, D., Kabir, A., Locatelli, M., and Samanidou, V. (2018). Food sample preparation for the determination of sulfonamides by high-performance liquid chromatography: State-of-the-art. Separations, 5.","DOI":"10.3390\/separations5020031"},{"key":"ref_35","unstructured":"AOAC International (2024, November 08). Method Validation Programs (OMA\/PVM Department), Including Appendix D: Guidelines for Collaborative Study Procedures to Validate Characteristics of a Method of Analysis. Available online: https:\/\/www.aoac.org\/."},{"key":"ref_36","doi-asserted-by":"crossref","first-page":"12","DOI":"10.1016\/j.envres.2019.03.021","article-title":"Comprehensive study of sulfamethoxazole effects in marine mussels: Bioconcentration, enzymatic activities and metabolomics","volume":"173","year":"2019","journal-title":"Environ. Res."},{"key":"ref_37","unstructured":"DrugBank Online (2024, October 05). Database for Drug and Drug Target Info. Available online: https:\/\/go.drugbank.com\/."},{"key":"ref_38","unstructured":"Chemical BooK (2024, October 05). Sourcing and Integrating Center of Chemicals Materials in China. Available online: https:\/\/www.chemicalbook.com\/."},{"key":"ref_39","doi-asserted-by":"crossref","first-page":"906","DOI":"10.1016\/j.scitotenv.2017.09.328","article-title":"A duodecennial national synthesis of antibiotics in China\u2019s major rivers and seas (2005\u20132016)","volume":"615","author":"Li","year":"2018","journal-title":"Sci. Total Environ."},{"key":"ref_40","doi-asserted-by":"crossref","first-page":"6625","DOI":"10.1007\/s00216-019-02035-2","article-title":"Routine analytical method for monitoring the main metabolites for a recurrent group of parabens and pharmaceuticals in wastewater and tap water","volume":"411","author":"Malvar","year":"2019","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_41","doi-asserted-by":"crossref","first-page":"639","DOI":"10.3181\/00379727-97-23830","article-title":"Chemotherapeutic Activity of Some Sulfapyridine-1-Oxides","volume":"97","author":"Scudi","year":"1958","journal-title":"Proc. Soc. Exp. Biol. Med."},{"key":"ref_42","doi-asserted-by":"crossref","first-page":"815","DOI":"10.1016\/j.scitotenv.2018.10.417","article-title":"Trace determination of sulfonamide antibiotics and their acetylated metabolites via SPE-LC-MS\/MS in wastewater and insights from their occurrence in a municipal wastewater treatment plant","volume":"653","author":"Yuan","year":"2019","journal-title":"Sci. Total Environ."},{"key":"ref_43","doi-asserted-by":"crossref","first-page":"3373","DOI":"10.1007\/s00216-022-03953-4","article-title":"Development and validation of a highly effective analytical method for the evaluation of exposure of migratory birds to antibiotics and their metabolites by faeces analysis","volume":"414","author":"Santos","year":"2022","journal-title":"Anal. Bioanal. Chem."}],"container-title":["Molecules"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1420-3049\/29\/22\/5478\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,10]],"date-time":"2025-10-10T16:36:04Z","timestamp":1760114164000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1420-3049\/29\/22\/5478"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2024,11,20]]},"references-count":43,"journal-issue":{"issue":"22","published-online":{"date-parts":[[2024,11]]}},"alternative-id":["molecules29225478"],"URL":"https:\/\/doi.org\/10.3390\/molecules29225478","relation":{},"ISSN":["1420-3049"],"issn-type":[{"value":"1420-3049","type":"electronic"}],"subject":[],"published":{"date-parts":[[2024,11,20]]}}}