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

Author(s)

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

Affiliation

^[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

• Document type: Journal article
• Source: ANALYTICAL AND BIOANALYTICAL CHEMISTRY; v. 413, n. 20, SI, p. 5147-5160, AUG 2021.
• Web of Science Citations: 0

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 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)

• FAPESP's process: 18/11700-7 - Determination of pharmaceuticals in wastewater
• Grantee: César Augusto Marasco Júnior
• Support Opportunities: Scholarships in Brazil - Master
• FAPESP's process: 14/50945-4 - INCT 2014: National Institute for Alternative Technologies of Detection, Toxicological Evaluation and Removal of Micropollutants and Radioactivies
• Grantee: Maria Valnice Boldrin
• Support Opportunities: Research Projects - Thematic Grants
• FAPESP's process: 18/22393-8 - Biochar applied in the removal of emerging contaminants present in wastewater
• Grantee: Paulo Clairmont Feitosa de Lima Gomes
• Support Opportunities: Regular Research Grants
• FAPESP's process: 16/03369-3 - Development of paper-based microfluidic devices for pharmaceuticas analysis in wastewaters.
• Grantee: Paulo Clairmont Feitosa de Lima Gomes
• Support Opportunities: Regular Research Grants