Analysis of highly polar marine biotoxins in seawater by hydrophilic interaction liquid chromatography coupled to high resolution mass spectrometry

The monitoring of marine biotoxins (MBTs) in seawater is presented as an alternative strategy to determine their presence and the possible implications in the ecosystem. For this, an analytical method based on hydrophilic interaction liquid chromatography coupled to high resolution mass spectrometry (HILIC-HRMS) has been developed to identify and quantify some hydrophilic MBTs in seawater: saxitoxin (STX), decarbamoyl-saxitoxin (dcSTX), neosaxitoxin (NeoSTX), gonaytoxin-2,3 (GTX-2,3) and tetrodotoxin (TTX), which are responsible of gastrointestinal and central nervous system distress in humans when are consumed via seafood. Particulate and filtrate portion were analyzed separately in order to characterize the extracellular toxins dissolved in the water and those present in the particulate. Ultrasound assisted solid-liquid extraction with methanol was used for the isolation of the MBTs from particulate and solid phase extraction using silica cartridges for the filtrate. Extraction procedure was the most critical step during the analytical method due to the high polarity of the toxins and the absolute recoveries obtained ranged from 15 to 47 % in the filtrate and 26 to 71 % in the particulate portions. Limits of detection of the method ranged from 0.5 to 5 µg/L in the filtrate portion and from 3.1 to 62 µg/L in the particulate portion.•Saxitoxins and tetrodotoxins have been analysed by using HILIC-HRMS.•UAE with methanol and SPE with silica cartridges have been employed for the extractions of the polar MBTs from seawater.

The work was supported by the Spanish Ministry of Economy and competitiveness through the project PLAS-MED (CTM2017-89701C3-1-R). The authors would like to express their deepest gratitude to Dr. Roser Chaler and Dori Fanjul, because of their technical support during the HPLC-HRMS analyses.

Peer reviewed