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. 2023 Aug 26;15(9):526.
doi: 10.3390/toxins15090526.

Measuring Marine Biotoxins in a Hypersaline Coastal Lagoon

Ainhoa Oller-Ruiz  1 , Nuria Alcaraz-Oliver  1 , Gema Férez  1 , Javier Gilabert  1
Affiliations

Measuring Marine Biotoxins in a Hypersaline Coastal Lagoon

Ainhoa Oller-Ruiz et al. Toxins (Basel). .

Abstract

Marine biotoxins have posed a persistent problem along various coasts for many years. Coastal lagoons are ecosystems prone to phytoplankton blooms when altered by eutrophication. The Mar Menor is the largest hypersaline coastal lagoon in Europe. Sixteen marine toxins, including lipophilic toxins, yessotoxins, and domoic acid (DA), in seawater samples from the Mar Menor coastal lagoon were measured in one year. Only DA was detected in the range of 44.9-173.8 ng L-1. Environmental stressors and mechanisms controlling the presence of DA in the lagoon are discussed. As an enrichment and clean-up method, we employed solid phase extraction to filter and acidify 75 mL of the sample, followed by pre-concentration through a C18 SPE cartridge. The analytes were recovered in aqueous solutions and directly injected into the liquid chromatography system (LC-MS), which was equipped with a C18 column. The system operated in gradient mode, and we used tandem mass spectrometry (MS/MS) with a triple quadrupole (QqQ) in the multiple reaction monitoring mode (MRM) for analysis. The absence of matrix effects was checked and the limits of detection for most toxins were low, ranging from 0.05 to 91.2 ng L-1, depending on the compound. To validate the measurements, we performed recovery studies, falling in the range of 74-122%, with an intraday precision below 14.9% RSD.

Keywords: Mar Menor; coastal lagoons; liquid chromatography; marine toxins; solid phase extraction; triple quadrupole mass spectrometry.

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Conflict of interest statement

The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

Figures

Figure 1
Figure 1
Elution solvents tested in SPE extraction of domoic acid: (A) study of methanol percentage; (B) study of basic solutions.
Figure 2
Figure 2
Elution solvents in SPE extraction of lipophilic toxins and yessotoxins tested: (A,B) study of percentage of methanol; (C,D) study of basic solutions.
Figure 3
Figure 3
Time series overlap of Pseudo-nitzschia density (blue diamonds), domoic acid concentration (pale green bars), silicates to phosphates (Si:P) ratio (red dots and line), precipitation (grey bars from above), and salinity (dark cyan dosts and line) in the Mar Menor lagoon. The water DA concentrations can be explained by a trade-off of bottom-up and top-down factors. Bottom-up factors are characterized by the Si:P ratio as a proxy for nutrients limitation; top-down factors are mainly dilution factor due to precipitation (as a proxy of rain over the lagoon plus run-off of the catchment area) and salinity as a proxy for the exchange of water with the Mediterranean Sea, mainly through the Encañizadas inlet. These factors, together with advection processes, explain the poor correlation between Pseudo-nitzschia density and DA concentration.
Figure 4
Figure 4
Locations of the Mar Menor coastal lagoon, sampling station, and meteorological station with detail of the three inlets connecting the Mar Menor coastal lagoon with the Mediterranean Sea. The cross-sectional area of the Las Encañizadas inlet is 40% of the total cross-sectional area of the lagoon, which has a heavy influence on the water exchange at the sampling point.
See this image and copyright information in PMC

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