Work

Targeted and untargeted approaches using liquid chromatography with high-resolution mass spectrometry for the determination of lipophilic marine biotoxins in seawater and mussel samples

Year: 2025

Type: article

Abstract: Marine biotoxins are naturally occurring compounds produced around the world by various species of microalgae, whose presence increases significantly due to harmful algal blooms. This phenomenon is a major public health concern, as a large amount of marine fauna is exposed to these biotoxins. The aim of this study was the improvement and application of dispersive liquid-liquid microextraction and liquid chromatography coupled to high-resolution mass spectrometry for the determination of eight lipophilic marine biotoxins, okadaic acid (OA), dinophysistoxin 1 (DTX-1), dinophysistoxin 2 (DTX-2), 16:0 7-O-acyl okadaic acid (DTX-3a), gambierone (GAM), 44-methylgambierone (44-GAM), yessotoxin (YTX), and homoyessotoxin (hYTX), and their derivatives in seawaters and mussels by targeted and untargeted approaches. The proposed method provided detection limits ranging from 0.0004 to 1.7 ng mL −1 in seawater and 0.06 to 119 ng g −1 in mussel samples, depending on the biotoxin. A total of 23 seawater samples collected in the Mar Menor lagoon between 2021 and 2023 were analyzed and several of them were found to contain OA and DTX-3a at concentration levels in the 0.006–1.5 ng mL −1 range. OA and DTX-2 were also found at maximum levels of 8.0 and 1.2 ng g −1 , respectively, in several mussel samples from commercial origin. In addition, a suspect screening was developed in the untargeted approach to investigate the presence of other derivatives of the target marine biotoxins in the samples using a home-made database covering 93 compounds. An unsaturated ester derivative of OA/DTX-2 was detected in the seawater samples collected during a red tide. • Analysis of lipophilic biotoxins in seawater from an eutrophicated zone • The environmentally friendly DLLME step allowed a sensitive detection of biotoxins. • Suspect screening allowed the search of lipophilic biotoxin congeners. • OA, DTX-2 and ester derivatives were found in several samples.

Source: Marine Pollution Bulletin

DOI: 10.1016/j.marpolbul.2025.118688