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Automated method to determine pharmaceutical compounds in wastewater using on-line solid-phase extraction coupled to LC-MS/MS

dc.contributor.authorMarasco Júnior, César Augusto [UNESP]
dc.contributor.authorda Silva, Bianca Ferreira [UNESP]
dc.contributor.authorLamarca, Rafaela Silva [UNESP]
dc.contributor.authorde Lima Gomes, Paulo Clairmont Feitosa [UNESP]
dc.contributor.institutionUniversidade Estadual Paulista (UNESP)
dc.contributor.institutionUniversity of Florida
dc.date.accessioned2022-04-28T19:40:56Z
dc.date.available2022-04-28T19:40:56Z
dc.date.issued2021-08-01
dc.description.abstractAn automated method was developed using on-line solid-phase extraction (SPE) as a sample preparation step, coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS), for determination of pharmaceutical compounds in wastewater samples at nanograms per liter to micrograms per liter concentration levels. This method is suitable for use in routine analysis, especially in environmental applications, avoiding cross-contamination and requiring minimal sample handling. Results can be obtained rapidly, with a chromatographic run time of only 24 min (including sample preparation and chromatographic analysis). Using a 50 μL injection volume, the method was validated according to international guidelines, considering parameters included in terms of method detection (MDL) and quantification limit (MQL), linearity, inter-day and intra-day precisions, and matrix effects. Assessment of chromatographic efficiency considered peak resolution and asymmetry, and carryover was evaluated to ensure analytical reliability and the ability to reuse the SPE cartridge. The intra- and inter-day precisions were lower than 10 and 17%, respectively. The MDL values ranged from 1×10-6 to 1 μg L-1, while the MQL values were from 0.001 to 3 μg L-1. Matrix effects were minimized by isotope dilution calibration. Application of the method to 20 wastewater samples showed that caffeine was the most frequently detected compound, with the highest concentration of 715 μg L-1, while other pharmaceutical compounds were detected in fewer samples and at lower concentrations (up to 8.51 μg L-1). Graphical abstract: [Figure not available: see fulltext.]en
dc.description.affiliationNational Institute for Alternative Technologies of Detection Toxicological Evaluation and Removal of Micropollutants and Radioactives (INCT-DATREM) Institute of Chemistry São Paulo State University, P.O. Box 355
dc.description.affiliationCollege of Veterinary Medicine Department of Physiological Sciences University of Florida, P.O. Box 490
dc.description.affiliationUnespNational Institute for Alternative Technologies of Detection Toxicological Evaluation and Removal of Micropollutants and Radioactives (INCT-DATREM) Institute of Chemistry São Paulo State University, P.O. Box 355
dc.description.sponsorshipFundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
dc.description.sponsorshipConselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
dc.description.sponsorshipCoordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
dc.description.sponsorshipIdFAPESP: #18/11700-7
dc.description.sponsorshipIdFAPESP: #18/2239
dc.description.sponsorshipIdCNPq: #465571/2014-0
dc.description.sponsorshipIdCAPES: #88887136426/2017/00
dc.description.sponsorshipIdFAPESP: grants #16/03369-3
dc.format.extent5147-5160
dc.identifierhttp://dx.doi.org/10.1007/s00216-021-03481-7
dc.identifier.citationAnalytical and Bioanalytical Chemistry, v. 413, n. 20, p. 5147-5160, 2021.
dc.identifier.doi10.1007/s00216-021-03481-7
dc.identifier.issn1618-2650
dc.identifier.issn1618-2642
dc.identifier.scopus2-s2.0-85108791034
dc.identifier.urihttp://hdl.handle.net/11449/221848
dc.language.isoeng
dc.relation.ispartofAnalytical and Bioanalytical Chemistry
dc.sourceScopus
dc.subjectEmerging contaminants
dc.subjectLiquid chromatography-tandem mass spectrometry
dc.subjectOn-line sample preparation
dc.subjectPharmaceutical compounds
dc.subjectWastewater analysis
dc.titleAutomated method to determine pharmaceutical compounds in wastewater using on-line solid-phase extraction coupled to LC-MS/MSen
dc.typeArtigopt
dspace.entity.typePublication
relation.isOrgUnitOfPublicationbc74a1ce-4c4c-4dad-8378-83962d76c4fd
relation.isOrgUnitOfPublication.latestForDiscoverybc74a1ce-4c4c-4dad-8378-83962d76c4fd
unesp.author.orcid0000-0003-0454-3419[1]
unesp.author.orcid0000-0002-5517-6666[2]
unesp.author.orcid0000-0002-8605-8013[3]
unesp.author.orcid0000-0002-4837-6352[4]
unesp.campusUniversidade Estadual Paulista (UNESP), Instituto de Química, Araraquarapt

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