Automated method to determine pharmaceutical compounds in wastewater using on-line solid-phase extraction coupled to LC-MS/MS
dc.contributor.author | Marasco Júnior, César Augusto [UNESP] | |
dc.contributor.author | da Silva, Bianca Ferreira [UNESP] | |
dc.contributor.author | Lamarca, Rafaela Silva [UNESP] | |
dc.contributor.author | de Lima Gomes, Paulo Clairmont Feitosa [UNESP] | |
dc.contributor.institution | Universidade Estadual Paulista (UNESP) | |
dc.contributor.institution | University of Florida | |
dc.date.accessioned | 2022-04-28T19:40:56Z | |
dc.date.available | 2022-04-28T19:40:56Z | |
dc.date.issued | 2021-08-01 | |
dc.description.abstract | An 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.affiliation | National 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.affiliation | College of Veterinary Medicine Department of Physiological Sciences University of Florida, P.O. Box 490 | |
dc.description.affiliationUnesp | National 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.sponsorship | Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) | |
dc.description.sponsorship | Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) | |
dc.description.sponsorship | Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) | |
dc.description.sponsorshipId | FAPESP: #18/11700-7 | |
dc.description.sponsorshipId | FAPESP: #18/2239 | |
dc.description.sponsorshipId | CNPq: #465571/2014-0 | |
dc.description.sponsorshipId | CAPES: #88887136426/2017/00 | |
dc.description.sponsorshipId | FAPESP: grants #16/03369-3 | |
dc.format.extent | 5147-5160 | |
dc.identifier | http://dx.doi.org/10.1007/s00216-021-03481-7 | |
dc.identifier.citation | Analytical and Bioanalytical Chemistry, v. 413, n. 20, p. 5147-5160, 2021. | |
dc.identifier.doi | 10.1007/s00216-021-03481-7 | |
dc.identifier.issn | 1618-2650 | |
dc.identifier.issn | 1618-2642 | |
dc.identifier.scopus | 2-s2.0-85108791034 | |
dc.identifier.uri | http://hdl.handle.net/11449/221848 | |
dc.language.iso | eng | |
dc.relation.ispartof | Analytical and Bioanalytical Chemistry | |
dc.source | Scopus | |
dc.subject | Emerging contaminants | |
dc.subject | Liquid chromatography-tandem mass spectrometry | |
dc.subject | On-line sample preparation | |
dc.subject | Pharmaceutical compounds | |
dc.subject | Wastewater analysis | |
dc.title | Automated method to determine pharmaceutical compounds in wastewater using on-line solid-phase extraction coupled to LC-MS/MS | en |
dc.type | Artigo | pt |
dspace.entity.type | Publication | |
relation.isOrgUnitOfPublication | bc74a1ce-4c4c-4dad-8378-83962d76c4fd | |
relation.isOrgUnitOfPublication.latestForDiscovery | bc74a1ce-4c4c-4dad-8378-83962d76c4fd | |
unesp.author.orcid | 0000-0003-0454-3419[1] | |
unesp.author.orcid | 0000-0002-5517-6666[2] | |
unesp.author.orcid | 0000-0002-8605-8013[3] | |
unesp.author.orcid | 0000-0002-4837-6352[4] | |
unesp.campus | Universidade Estadual Paulista (UNESP), Instituto de Química, Araraquara | pt |