A new on-line SPE LC-HRMS method for simultaneous analysis of selected emerging contaminants in surface waters?

Analytical Methods Pub Date: 2022-12-16 DOI: 10.1039/D2AY01574A

Abstract

In recent years emerging contaminants (ECs) have received significant attention due to their widespread detection in surface waters and concerns that these compounds can cause adverse ecological and/or human health effects. Therefore, accurate methods for determining and quantifying ECs in surface water are essential for estimating their environmental impact. This work describes the development, validation and application of a sensitive multiclass method for simultaneous determination of 22 per and polyfluorinated alkyl substances (PFASs), 3 pharmaceuticals, 15 pesticides, and 2 bisphenols in surface water using on-line solid phase extraction (SPE) coupled with ultra-performance liquid chromatography-high-resolution mass spectrometry (UPLC-HRMS). The method allows simultaneous sample clean-up from interfering matrices and lower limits of detection (LODs) by injecting a large sample volume into the LC system without compromising chromatographic efficiency and resolution. Linearity of response over several orders of magnitude was demonstrated for all tested compounds (R2 > 0.99), with the LODs ranging from 0.8 and 33.7 pg mL?1, allowing detection of ECs at trace levels in surface water. The method showed acceptable accuracy and precision (CV, % and RE below 20%) for all tested ECs. It also provided recoveries between 60% and 130% for all tested ECs. The validated method was successfully applied for analysis of surface water samples from three rivers (Cam, Ouse and Thames) in England. Several ECs, including perfluorooctanesulfonic acid (PFOS), perfluorobutanesulfonic acid (PFBS), perfluorohexanoic acid (PFHxA), perfluorohexane sulfonic acid (PFHxS), dimethyl-metatoluamide (DEET) and ibuprofen were observed in analysed surface water above the method's limit of quantitation (LOQ), with concentrations ranging between 3.5 and 460 pg mL?1.

Graphical abstract: A new on-line SPE LC-HRMS method for simultaneous analysis of selected emerging contaminants in surface waters
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