Dataset Information

Ultra-Trace Analysis of Cyanotoxins by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry.

ABSTRACT: The increasing frequency of episodes of harmful algal blooms of cyanobacterial origin is a risk to ecosystems and human health. The main human hazard may arise from drinking water supply and recreational water use. For this reason, efficient multiclass analytical methods are needed to assess the level of cyanotoxins in water reservoirs and tackle these problems. This work describes the development of a fast, sensitive, and robust analytical method for multiclass cyanotoxins determination based on dual solid-phase extraction (SPE) procedure using a polymeric cartridge, Oasis HLB (Waters Corporation, Milford, MA, USA), and a graphitized non-porous carbon cartridge, SupelcleanTM ENVI-CarbTM (Sigma-Aldrich, St. Louis, MO, USA), followed by ultra-high-performance liquid chromatography high-resolution mass spectrometry (SPE-UHPLC-HRMS). This method enabled the analysis of cylindrospermopsin, anatoxin-a, nodularin, and seven microcystins (MC-LR, MC-RR, MC-YR, MC-LA, MC-LY, MC-LW, MC-LF). The method limits of detection (MLOD) of the validated approach were between 4 and 150 pg/L. The analytical method was applied to assess the presence of the selected toxins in 21 samples collected in three natural water reservoirs in the Ter River in Catalonia (NE of Spain) used to produce drinking water for Barcelona city (Spain).

SUBMITTER: Filatova D

PROVIDER: S-EPMC7232229 | biostudies-literature | 2020 Apr

REPOSITORIES: biostudies-literature

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Ultra-Trace Analysis of Cyanotoxins by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry.

Filatova Daria D Núñez Oscar O Farré Marinella M

Toxins 20200411 4

The increasing frequency of episodes of harmful algal blooms of cyanobacterial origin is a risk to ecosystems and human health. The main human hazard may arise from drinking water supply and recreational water use. For this reason, efficient multiclass analytical methods are needed to assess the level of cyanotoxins in water reservoirs and tackle these problems. This work describes the development of a fast, sensitive, and robust analytical method for multiclass cyanotoxins determination based o ...[more]

PMID: 32290413

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Project description:BackgroundThe widespread utilization of organic compounds in modern society and their dispersion through wastewater have resulted in extensive contamination of source and drinking waters. The vast majority of these compounds are not regulated in wastewater outfalls or in drinking water while trace amounts of certain compounds can impact aquatic wildlife. Hence it is prudent to monitor these contaminants in water sources until sufficient toxicological data relevant to humans becomes available. A method was developed for the analysis of 36 trace organic contaminants (TOrCs) including pharmaceuticals, pesticides, steroid hormones (androgens, progestins, and glucocorticoids), personal care products and polyfluorinated compounds (PFCs) using a single solid phase extraction (SPE) technique with ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). The method was applied to a variety of water matrices to demonstrate method performance and reliability.ResultsUHPLC-MS/MS in both positive and negative electrospray ionization (ESI) modes was employed to achieve optimum sensitivity while reducing sample analysis time (<20 min) compared with previously published methods. The detection limits for most compounds was lower than 1.0 picogram on the column while reporting limits in water ranged from 0.1 to 15 ng/L based on the extraction of a 1 L sample and concentration to 1 mL. Recoveries in ultrapure water for most compounds were between 90-110%, while recoveries in surface water and wastewater were in the range of 39-121% and 38-141% respectively. The analytical method was successfully applied to analyze samples across several different water matrices including wastewater, groundwater, surface water and drinking water at different stages of the treatment. Among several compounds detected in wastewater, sucralose and TCPP showed the highest concentrations.ConclusionThe proposed method is sensitive, rapid and robust; hence it can be used to analyze a large variety of trace organic compounds in different water matrixes.

Project description:The knowledge about the molecular fraction contributing to white wines oxidative stability is still poorly understood. However, the role of S- and N-containing compounds, like glutathione and other peptides, as a source of reductant in many oxidation reactions, and acting against heavy metals toxicity, or lipid and polyphenol oxidation as ROS-scavenger is today very well established. In that respect, the aim of the present study is to introduce an original analytical tool for the direct determination of the available nucleophilic compounds in white wine under acidic pH conditions. One step derivatization of nucleophiles has been realized directly in wines using 4-methyl-1,2-benzoquinone (4MeQ) as an electrophilic probe. Derivatization conditions considering probe concentration, pH, reaction time, MS ionisation conditions and adducts stability, were optimized using model solutions containing standard sulfur and amino compounds (GSH, Cys, HCys and Ser-Aps-Cys-Asp-Ser, Asp-Met, Met and Glu). Ultra-high-performance liquid chromatography coupled to a quadrupole-time of flight mass spectrometer (UHPLC-QqTOF-MS) analysis of up to 92 white wines from different cultivars (Chardonnay, Sauvignon and Semillon) followed by Multivariate analysis (PLS DA) and Wilcoxon test allowed to isolate up to 141 putative wine relevant nucleophiles. Only 20 of these compounds, essentially thiols, were detectable in samples before derivatization, indicating the importance of the quinone trapping on the revelation of wine unknown nucleophiles. Moreover, annotation using online database (Oligonet, Metlin and KEGG) as well as elementary formula determined by isotopic profile, provided evidence of the presence of amino acids (Val, Leu, Ile, Pro, Trp, Cys and Met) and peptides with important antioxidant properties. The complimentary set of MS/MS spectral data greatly accelerated identification of nucleophiles and enabled peptides sequencing. These results show that probing wines with 4-methyl-1,2-benzoquinone enhances thiols ionisation capacity and gives a better screening of specific S- N- containing functional compounds as part of the white wines antioxidant metabolome.

Dataset Information

Ultra-Trace Analysis of Cyanotoxins by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry.

Publications

Ultra-Trace Analysis of Cyanotoxins by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry.

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