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Title: Method Development for Comprehensive Extraction and Analysis of Marine Toxins: Liquid-Liquid Extraction and Tandem Liquid Chromatography Separations Coupled to Electrospray Tandem Mass Spectrometry

Abstract

A variety of toxins are produced by marine and freshwater microorganisms that present a threat to human health. These toxins have diverse chemical properties and specifically, a range of hydrophobicity. Methods for extraction and identification of these toxins are often geared toward specific classes of toxin depending on the sample type. There is a need for a general method of toxin extraction and identification for screening samples where the likely toxin content is not known a priori. Here, we have applied a general method for metabolite extraction to toxin containing samples. This method was coupled with a simple dual liquid chromatography approach for separating a broad range of toxins. This liquid chromatography approach was coupled to triple quadrupole and quadrupole time-of-flight MS/MS platforms. The method was testing on a fish matrix for recovery of palytoxin as well as marine corals for detection of natural mixtures of palytoxin analogues. The recovery of palytoxin was found to produce a linear response (R2 of 0.95) when spiked into the fish matrix with a limit of quantitation of 2.5 ng/μL and recovery efficiency of 73% +/- 9%. The screening of corals revealed varying amount of palytoxin, and in one case, different palytoxin structural analogues.more » This demonstration illustrates the potential utility of this method for toxin extraction and detection.« less

Authors:
 [1];  [1];  [1];  [1];  [2]
+ Show Author Affiliations
  1. Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Chemical and Biological Signature Sciences
  2. Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Coastal Sciences
Publication Date:
Research Org.:
Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)
Sponsoring Org.:
USDOE; USDHS
OSTI Identifier:
1437020
Report Number(s):
PNNL-SA-131966
Journal ID: ISSN 0039-9140; PII: S0039914018304879
Grant/Contract Number:  
AC05-76RL01830; HSHQPM16X00100
Resource Type:
Accepted Manuscript
Journal Name:
Talanta
Additional Journal Information:
Journal Volume: 187; Journal ID: ISSN 0039-9140
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
59 BASIC BIOLOGICAL SCIENCES; Toxin profiling; Dual Column Liquid Chromatography; Hydrophilic Interaction; Reverse Phase; Triple Quadrupole; Quadrupole Time-of-Flight

Citation Formats

Wunschel, David S., Valenzuela, Blandina R., Kaiser, Brooke L. Deatherage, Victry, Kristin, and Woodruff, Dana. Method Development for Comprehensive Extraction and Analysis of Marine Toxins: Liquid-Liquid Extraction and Tandem Liquid Chromatography Separations Coupled to Electrospray Tandem Mass Spectrometry. United States: N. p., 2018. Web. doi:10.1016/j.talanta.2018.05.019.
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Wunschel, David S., Valenzuela, Blandina R., Kaiser, Brooke L. Deatherage, Victry, Kristin, & Woodruff, Dana. Method Development for Comprehensive Extraction and Analysis of Marine Toxins: Liquid-Liquid Extraction and Tandem Liquid Chromatography Separations Coupled to Electrospray Tandem Mass Spectrometry. United States. https://doi.org/10.1016/j.talanta.2018.05.019
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Wunschel, David S., Valenzuela, Blandina R., Kaiser, Brooke L. Deatherage, Victry, Kristin, and Woodruff, Dana. Wed . "Method Development for Comprehensive Extraction and Analysis of Marine Toxins: Liquid-Liquid Extraction and Tandem Liquid Chromatography Separations Coupled to Electrospray Tandem Mass Spectrometry". United States. https://doi.org/10.1016/j.talanta.2018.05.019. https://www.osti.gov/servlets/purl/1437020.
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@article{osti_1437020,
title = {Method Development for Comprehensive Extraction and Analysis of Marine Toxins: Liquid-Liquid Extraction and Tandem Liquid Chromatography Separations Coupled to Electrospray Tandem Mass Spectrometry},
author = {Wunschel, David S. and Valenzuela, Blandina R. and Kaiser, Brooke L. Deatherage and Victry, Kristin and Woodruff, Dana},
abstractNote = {A variety of toxins are produced by marine and freshwater microorganisms that present a threat to human health. These toxins have diverse chemical properties and specifically, a range of hydrophobicity. Methods for extraction and identification of these toxins are often geared toward specific classes of toxin depending on the sample type. There is a need for a general method of toxin extraction and identification for screening samples where the likely toxin content is not known a priori. Here, we have applied a general method for metabolite extraction to toxin containing samples. This method was coupled with a simple dual liquid chromatography approach for separating a broad range of toxins. This liquid chromatography approach was coupled to triple quadrupole and quadrupole time-of-flight MS/MS platforms. The method was testing on a fish matrix for recovery of palytoxin as well as marine corals for detection of natural mixtures of palytoxin analogues. The recovery of palytoxin was found to produce a linear response (R2 of 0.95) when spiked into the fish matrix with a limit of quantitation of 2.5 ng/μL and recovery efficiency of 73% +/- 9%. The screening of corals revealed varying amount of palytoxin, and in one case, different palytoxin structural analogues. This demonstration illustrates the potential utility of this method for toxin extraction and detection.},
doi = {10.1016/j.talanta.2018.05.019},
journal = {Talanta},
number = ,
volume = 187,
place = {United States},
year = {Wed May 09 00:00:00 EDT 2018},
month = {Wed May 09 00:00:00 EDT 2018}
}
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Publisher's Version of Record
https://doi.org/10.1016/j.talanta.2018.05.019
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Works referenced in this record:

Investigation of the toxin profile of Greek mussels Mytilus galloprovincialis by liquid chromatography—mass spectrometry
journal, February 2006

Ovatoxin-a and Palytoxin Accumulation in Seafood in Relation to Ostreopsis cf. ovata Blooms on the French Mediterranean Coast
journal, February 2012

  • Amzil, Zouher; Sibat, Manoella; Chomerat, Nicolas
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Biosynthesis of anatoxin-a and analogues (anatoxins) in cyanobacteria
journal, December 2014

Detection of Saxitoxin-Producing Cyanobacteria and Anabaena circinalis in Environmental Water Blooms by Quantitative PCR
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  • Environmental Science & Technology, Vol. 47, Issue 8
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First Finding of Ostreopsis cf. ovata Toxins in Marine Aerosols
journal, March 2014

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  • Environmental Science & Technology, Vol. 48, Issue 6
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Liquid chromatography–high-resolution mass spectrometry for palytoxins in mussels
journal, December 2014

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  • Analytical and Bioanalytical Chemistry, Vol. 407, Issue 5
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Palytoxin Found in Palythoa sp. Zoanthids (Anthozoa, Hexacorallia) Sold in the Home Aquarium Trade
journal, April 2011

LC/MS analysis of brevetoxin metabolites in the Eastern oyster (Crassostrea virginica)
journal, March 2004

MPLEx: a Robust and Universal Protocol for Single-Sample Integrative Proteomic, Metabolomic, and Lipidomic Analyses
journal, May 2016

Preparation of Lipide Extracts from Brain Tissue
journal, August 1951

Determination of Palytoxins in Soft Coral and Seawater from a Home Aquarium. Comparison between Palythoa - and Ostreopsis -Related Inhalatory Poisonings
journal, December 2015

  • Tartaglione, Luciana; Dell’Aversano, Carmela; Mazzeo, Antonia
  • Environmental Science & Technology, Vol. 50, Issue 2
  • DOI: 10.1021/acs.est.5b05469

High Resolution LC-MSn Fragmentation Pattern of Palytoxin as Template to Gain New Insights into Ovatoxin-a Structure. The Key Role of Calcium in MS Behavior of Palytoxins
journal, February 2012

  • Ciminiello, Patrizia; Dell’Aversano, Carmela; Dello Iacovo, Emma
  • Journal of The American Society for Mass Spectrometry, Vol. 23, Issue 5
  • DOI: 10.1007/s13361-012-0345-7
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    Works referencing / citing this record:

    A Novel Sensitive Cell-Based Immunoenzymatic Assay for Palytoxin Quantitation in Mussels
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    A Novel Sensitive Cell-Based Immunoenzymatic Assay for Palytoxin Quantitation in Mussels
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    Development of an Efficient Extraction Method for Harvesting Gymnodimine-A from Large-Scale Cultures of Karenia selliformis
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