Complementarity of two approaches based on the use of high-resolution mass spectrometry for the determination of multi-class antibiotics in water. Photodegradation studies and non-target screenings

Abstract

The development of analytical methodologies to monitor different antibiotic families in water and the implementation of alternatives for their efficient elimination are a great challenge. The aim of this research was to develop a method based on solid-phase extraction followed by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry to analyse multi-class antibiotics, including macrolides, cephalosporins, fluoroquinolones, sulfonamides and diaminopyrimidines, in waters. Several parameters affecting the extraction such as the sample pH, type of sorbent and cartridge, elution volume and breakthrough volume were optimized. The method was validated in real samples, and matrix effect was assessed, demonstrating that the use of isotopically labelled surrogate compounds was mandatory to avoid standard addition calibration for each individual samples. Urban and hospital wastewater samples, as well as natural waters, were analysed, confirming the presence of 12 of the 14 target compounds at concentrations up to 3.5 µg L−1. Non-target analysis based on data-independent workflow was also performed, enabling the identification of 94 pollutants. Preliminary photodegradation experiments were also assessed, revealing the total removal of many target compounds after the first 5–10 min of UVC irradiation. In addition, 20 by-products formed after photolysis could be identified using a non-target approach.

Non-target screening in water analysis: recent trends of data evaluation, quality assurance, and their future perspectives

“…The use of NTS in advanced oxidation processes (AOPs) is on the rise. It offers several advantages, including the identification of unknown transformation products (TPs), understanding how the water matrix influences the formation of new TPs, determining treatment efficiency on a global scale, detecting abnormalities early, optimizing processes, and making decisions [5,53]. Furthermore, it was found that AOP treatment evaluation can be improved by adding supercritical fluid chromatography (SFC)-HRMS to the LC-HRMS-based workflow for identifying unknown persistent and mobile organic compounds (PMOCs) found in groundwater samples to achieve greater detection coverage of highly polar compounds [54].…”

An integrated framework to develop an efficient valid green (EVG) HPLC method for the assessment of antimicrobial pollutants with potential threats to human health in aquatic systems

“…Additionally, higher extraction recoveries and lower matrix effects were reported when compared to traditional SPE, as it removes the species responsible for such matrix effects. 42 According to previously reported methods, 43,44 methanol was the appropriate solvent for the elution of those drugs, but in accordance with green analytical chemistry, various water ratios were added to methanol. The ratio of water: methanol (20 : 80, v/v) nearly showed similar results as 100% methanol elution solvent.…”