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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

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 (R 2 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 structuralmore » analogues. This demonstration illustrates the potential utility of this method for toxin extraction and detection.« less
 [1] ;  [1] ;  [1] ;  [1] ;  [2]
  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:
Report Number(s):
PNNL-SA-131966; PNNL-SA-134603
Journal ID: ISSN 0039-9140; PII: S0039914018304879
Grant/Contract Number:
AC05-76RL01830; HSHQPM16X00100
Accepted Manuscript
Journal Name:
Additional Journal Information:
Journal Name: Talanta; Journal ID: ISSN 0039-9140
Research Org:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Org:
Country of Publication:
United States
59 BASIC BIOLOGICAL SCIENCES; Toxin profiling; Dual Column Liquid Chromatography; Hydrophilic Interaction; Reverse Phase; Triple Quadrupole; Quadrupole Time-of-Flight
OSTI Identifier:
Alternate Identifier(s):
OSTI ID: 1437021