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

Autor(es)

Marasco Junior, Cesar Augusto ^[1] ; da Silva, Bianca Ferreira ^{[1, 2]} ; Lamarca, Rafaela Silva ^[1] ; Feitosa de Lima Gomes, Paulo Clairmont ^[1]

Afiliação do(s) autor(es)

^[1] Sao Paulo State Univ, Natl Inst Alternat Technol Detect Toxicol Evaluat, Inst Chem, POB 355, BR-14800060 Araraquara, SP - Brazil

^[2] Univ Florida, Coll Vet Med, Dept Physiol Sci, POB 490, Gainesville, FL 32601 - USA

• Tipo de documento: Artigo Científico
• Fonte: ANALYTICAL AND BIOANALYTICAL CHEMISTRY; v. 413, n. 20, SI, p. 5147-5160, AUG 2021.
• Citações Web of Science: 0

Resumo

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 mu L 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 1x10(-6) to 1 mu g L-1, while the MQL values were from 0.001 to 3 mu g 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 mu g L-1, while other pharmaceutical compounds were detected in fewer samples and at lower concentrations (up to 8.51 mu g L-1). (AU)

• Processo FAPESP: 18/11700-7 - Determinação de fármacos em águas residuárias
• Beneficiário: César Augusto Marasco Júnior
• Modalidade de apoio: Bolsas no Brasil - Mestrado
• Processo FAPESP: 14/50945-4 - INCT 2014: Instituto Nacional de Tecnologias Alternativas para Detecção, Avaliação Toxicológica e Remoção de Micropoluentes e Radioativos
• Beneficiário: Maria Valnice Boldrin
• Modalidade de apoio: Auxílio à Pesquisa - Temático
• Processo FAPESP: 18/22393-8 - Biocarvão aplicado na remoção de contaminantes emergentes presentes em águas residuárias
• Beneficiário: Paulo Clairmont Feitosa de Lima Gomes
• Modalidade de apoio: Auxílio à Pesquisa - Regular
• Processo FAPESP: 16/03369-3 - Desenvolvimento de sistemas microfluídicos a base de papel aplicados na análise de fármacos em águas residuárias
• Beneficiário: Paulo Clairmont Feitosa de Lima Gomes
• Modalidade de apoio: Auxílio à Pesquisa - Regular