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Article

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

1
Virginia Institute of Marine Science, College of William & Mary, Gloucester Point, VA 23062, USA
2
Separation Technologies, Waters Corporation, Milford, MA 01757, USA
3
Institute of Marine and Environmental Technology, University of Maryland Center for Marine and Environmental Sciences, Baltimore, MD 21202, USA
*
Author to whom correspondence should be addressed.
Received: 24 March 2020 / Revised: 29 April 2020 / Accepted: 7 May 2020 / Published: 13 May 2020
(This article belongs to the Section Marine and Freshwater Toxins)
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. View Full-Text
Keywords: phycotoxins; mass spectrometry; UPLC-MS/MS; at-column dilution; SPATT; microcystins; okadaic acid; azaspiracids; pectenotoxins; brevetoxins phycotoxins; mass spectrometry; UPLC-MS/MS; at-column dilution; SPATT; microcystins; okadaic acid; azaspiracids; pectenotoxins; brevetoxins
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MDPI and ACS Style

Onofrio, M.D.; Mallet, C.R.; Place, A.R.; Smith, J.L. A Screening Tool for the Direct Analysis of Marine and Freshwater Phycotoxins in Organic SPATT Extracts from the Chesapeake Bay. Toxins 2020, 12, 322. https://0-doi-org.brum.beds.ac.uk/10.3390/toxins12050322

AMA Style

Onofrio MD, Mallet CR, Place AR, Smith JL. A Screening Tool for the Direct Analysis of Marine and Freshwater Phycotoxins in Organic SPATT Extracts from the Chesapeake Bay. Toxins. 2020; 12(5):322. https://0-doi-org.brum.beds.ac.uk/10.3390/toxins12050322

Chicago/Turabian Style

Onofrio, Michelle D., Claude R. Mallet, Allen R. Place, and Juliette L. Smith 2020. "A Screening Tool for the Direct Analysis of Marine and Freshwater Phycotoxins in Organic SPATT Extracts from the Chesapeake Bay" Toxins 12, no. 5: 322. https://0-doi-org.brum.beds.ac.uk/10.3390/toxins12050322

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