Automated microextraction by packed sorbent of endocrine disruptors in wastewater using a high-throughput robotic platform followed by liquid chromatography–tandem mass spectrometry

• Published in: Analytical and bioanalytical chemistry 2023-10, Vol.415 (25), p.6165-6176
• Main Authors: Bocelli, Marcio David, Medina, Deyber Arley Vargas, Lanças, Fernando Mauro, dos Santos-Neto, Álvaro José
• Format: Article
• Language: English
• Subjects: Analysis; Analytical Chemistry; Automation; Benzophenone; benzophenones; BHA; Biochemistry; Brazil; Butylated hydroxyanisole; Characterization and Evaluation of Materials; chemical species; Chemistry; Chemistry and Materials Science; Chromatography; Endocrine disruptors; Extraction (Chemistry); Food Science; Identification and classification; Laboratory Medicine; Liquid chromatography; Mass spectrometry; Mass spectroscopy; Mathematical analysis; Methods; methylparaben; microextraction; Monitoring/Environmental Analysis; Optimization; Phenolic compounds; Phenols; Propyl paraben; Research Paper; rivers; Robotics; robots; Scientific imaging; Sorbents; tandem mass spectrometry; Wastewater; Water analysis; Water monitoring; Water quality; Water quality management; Water sampling
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-023-04888-0

An automated microextraction by packed sorbent followed by liquid chromatography–tandem mass spectrometry (MEPS-LC–MS/MS) method was developed for the determination of four endocrine disruptors—parabens, benzophenones, and synthetic phenolic antioxidants—in wastewater samples. The method utilizes a lab-made repackable MEPS device and a multi-syringe robotic platform that provides flexibility to test small quantities (2 mg) of multiple extraction phases and enables high-throughput capabilities for efficient method development. The overall performance of the MEPS procedure, including the investigation of influencing variables and the optimization of operational parameters for the robotic platform, was comprehensively studied through univariate and multivariate experiments. Under optimized conditions, the target analytes were effectively extracted from a small sample volume of 1.5 mL, with competitive detectability and analytical confidence. The limits of detection ranged from 0.15 to 0.30 ng L −1 , and the intra-day and inter-day relative standard deviations were between 3 and 21%. The method’s applicability was successfully demonstrated by determining methylparaben, propylparaben, butylated hydroxyanisole, and oxybenzone in wastewater samples collected from the São Carlos (SP, Brazil) river. Overall, the developed method proved to be a fast, sensitive, reliable, and environmentally friendly analytical tool for water quality monitoring.