Determination of lipophilic marine biotoxins by liquid chromatography-tandem mass spectrometry in five shellfish species from Washington State, USA

Details

• Journal Title:
  Journal of Chromatography A
• Personal Author:
  Wang, Zhihong ; Doucette, Gregory J.
• NOAA Program & Office:
  NOS (National Ocean Service) ; NCCOS (National Centers for Coastal Ocean Science)
• Description:
  Low extraction efficiency (60-81%) of okadaic acid (OA) and dinophysistoxin 1 (DTX1) was obtained for 4 out of 5 shellfish species from Washington State (WA), USA, during application of a standard extraction method for determination of lipophilic marine biotoxins by LC-MS/MS as recommended by the European Union Reference Laboratory for Marine Biotoxins (EURLMB). OA and total OA including esters, DTX1, DTX2, and total DTX including esters, azaspiracid 1, 2, and 3 (AZA1, AZA2, and AZA3), pectenotoxin 2 (PTX2), and yessotoxin (YTX) were the toxins examined. Matrix-matched standards prepared from the same control samples used for spike-and-recovery tests were employed to evaluate toxin extraction efficiency and sample clean-up procedures. We adjusted the EURLMB extraction method by either using an acidified methanol extraction or pre-cooking shellfish homogenates at 70 °C for 20 min before EURLMB extraction. Extraction efficiency was improved markedly for OA and DTX1 with both modified methods and for YTX with the pre-cooking step included. However, recoveries were lower for YTX using the acidified methanol extraction and for PTX2 in non-mussel samples with the pre-cooking step. A hexane wash was applied to clean water-diluted non-hydrolyzed samples and a hexane wash was combined with solid-phase extraction for cleaning hydrolyzed samples. Improved sample clean-up, combined with LC-MS/MS adjustments, enabled quantification of U.S. Food and Drug Administration-regulated toxins in five shellfish species from WA with acceptable accuracy using non-matrix matched calibration standards.
• Keywords:
  Biotoxins Shellfishes
• Source:
  Journal of Chromatography A, 1639, 461902
• DOI:
  https://doi.org/10.1016/j.chroma.2021.461902
• ISSN:
  0021-9673
• Publisher:
  Elsevier BV
• Document Type:
  Journal Article
• Rights Information:
  Accepted Manuscript
• Rights Statement:
  This manuscript is made available under the Elsevier user license https://www.elsevier.com/open-access/userlicense/1.0/
• Compliance:
  Library
• Main Document Checksum:
  urn:sha256:a103fe0902e6b474ffe98499789a020e3eece256d8605290b8c6b67c47102830
• Download URL:
  https://repository.library.noaa.gov/view/noaa/50819/noaa_50819_DS1.pdf
• File Type:
  [PDF - 201.30 KB ]