Simultaneous Pre-Concentration and HPLC-MS/MS Quantification of Phycotoxins and Cyanotoxins in Inland and Coastal Waters

Abstract

<jats:p>The purpose of this study was to set up a sensitive method for the simultaneous determination of phycotoxins and cyanotoxins—Emerging pollutants with different structures and harmful properties (hepatotoxicity, neurotoxicity and cytotoxicity)—In environmental waters. Due to the low concentrations detected in these samples, a pre-concentration step is required and here it was performed in a single step with a commercial cartridge (Strata™-X), achieving enrichment factors up to 200 and satisfactory recovery (R = 70–118%) in different aqueous matrices. After solid-phase extraction (SPE), toxins were separated and quantified by High Performance Liquid Chromatography- Heated ElectroSpray Ionisation Tandem Mass Spectrometry (HPLC-HESI-MS/MS) in Multiple Reaction Monitoring (MRM) mode. An analytical evaluation of the proposed method was done based on the analytical figures of merit, such as precision and trueness, linearity, selectivity, and sensitivity, and it turned out to be a robust tool for the quantification of ng L−1 levels, phycotoxins and cyanotoxins in both freshwater and saltwater samples.</jats:p>

Substances of emerging concern in Baltic Sea water: Review on methodological advances for the environmental assessment and proposal for future monitoring

“…However, if higher enrichment factors are required, solid phase extraction (SPE) is the method of choice for UV filters (Bratkovics and Sapozhnikova 2011 ), pharmaceuticals (Paíga et al 2015 ; Białk-Bielińska et al 2016 ), pesticides (Loos et al 2013 ; Rodríguez-González et al 2017 ; Li et al 2019 ; Xiao et al 2021 ), estrogens (Rocha et al 2012 ; Ronan and McHugh 2013 ; Heub et al 2015 ), and PFAS (Loos et al 2013 ; Brumovský et al 2018 ). Besides classical off-line SPE approaches, automated procedures directly coupled to LC systems have been utilized in the last years, e.g., for the analysis of UV filters in seawater samples (Oliveira et al 2010 ; Montesdeoca-Esponda et al 2012 ), triazine herbicides (Rodríguez-González et al 2016 ), and algal toxins (Zhang et al 2018 ; Merlo et al 2020 ; Wang et al 2021 ).…”

Co-Occurrence of Cyanobacteria and Cyanotoxins with Other Environmental Health Hazards: Impacts and Implications

“…Following wildlife-, domestic animal-, and human-intoxications due to exposure to cyanobacterial mass populations, the volume of research over recent years into the toxicology and toxinology of cyanobacteria and cyanotoxins has increased greatly and such growth continues e.g., [ 1 , 5 , 7 , 8 ]. In recognition of the co-occurrence of multiple variants within individual classes of cyanotoxins, of different cyanotoxin classes, and of cyanotoxins plus phycotoxins, it is encouraging that physico-chemical methods for the co-analysis of these combinations are being developed [ 5 , 19 , 20 , 21 , 140 ]. However, since cyanobacterial mass populations commonly develop in waterbodies which are under intensive anthropogenic use (e.g., for domestic, industrial, and agricultural wastewater discharge, abstraction for drinking water treatment, recreation, crop irrigation, and fisheries) it should be anticipated that toxigenic cyanobacteria can co-occur with a wide range of additional biological and chemical health hazards.…”