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    A Screening Tool for the Direct Analysis of Marine and Freshwater Phycotoxins in Organic SPATT Extracts from the Chesapeake Bay

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    Author
    Onofrio, M.D.
    Mallet, C.R.
    Place, A.R.
    Date
    2020
    Journal
    Toxins
    Publisher
    MDPI, AG
    Type
    Article
    
    Metadata
    Show full item record
    See at
    https://doi.org/10.3390/toxins12050322
    Abstract
    Many detection methods for phycotoxins, bioactive compounds produced by harmful algae, focus on one compound or a class of related compounds. Multiple harmful algal species often co-occur in the environment, however, emphasizing the need to analyze for the presence of multiple groups of marine and freshwater phycotoxins in environmental samples, e.g., extracts from solid phase adsorption toxin tracking (SPATT). Two methods were developed to screen for 13 phycotoxins (microcystin-RR, -LR, -YR, azaspiracid-1, -2, karlotoxin 3, goniodomin A, brevetoxin-2, yessotoxin, pectenotoxin-2, dinophysistoxin-1, -2, and okadaic acid) in organic SPATT extracts using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) equipped with a trapping dimension (trap) and at-column dilution (ACD). The performance of each compound under 36 combinations of chromatographic conditions was characterized, and two final methods, acidic and basic, were selected based on peak shapes, signal intensities, resolution, and the separation in time of positive and negative MS ionization modes. Injection volumes of up to 1 mL were possible through trap/ACD technology, resulting in limits of detection between 0.001 and 0.05 µg/L across the analytes. Benefits highlighted in this study, beyond the improved detection limits and co-detection of multiple toxin groups, include the ability to inject samples of 100% organic solvent, ensuring analyte stability and streamlining workflow through the elimination of laborious sample preparation steps.
    Keyword
    at-column dilution
    azaspiracids
    brevetoxins
    mass spectrometry
    microcystins
    okadaic acid
    pectenotoxins
    phycotoxins
    SPATT
    UPLC-MS/MS
    Identifier to cite or link to this item
    https://www.scopus.com/inward/record.uri?eid=2-s2.0-85084786049&doi=10.3390%2ftoxins12050322&partnerID=40&md5=1a4563607598e2ebfd0e69f022200a78; http://hdl.handle.net/10713/12887
    ae974a485f413a2113503eed53cd6c53
    10.3390/toxins12050322
    Scopus Count
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    UMB Open Access Articles 2020

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