Measuring Marine Biotoxins in a Hypersaline Coastal Lagoon.

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.

Stir bar sorptive extraction coupled to liquid chromatography for the analysis of strobilurin fungicides in fruit samples.

A stir bar microextraction (SBSE) procedure for the determination of seven strobilurin fungicides in fruit samples using liquid chromatography (LC) and diode array detection (DAD) has been developed. The samples were sonicated in the presence of ethanol before submitting the extracts to SBSE. The incorporation of drazoxolon as an internal standard before SBSE allowed calibration without the need to use the standard additions method. Under the optimized conditions, detection limits were in the 0.3-2 ng g(-1) range, corresponding to trifloxystrobin and metominostrobin, respectively. The SBSE-LC-DAD procedure showed good repeatability (RSD below 11% in all cases) and provided recoveries of 80-105% from spiked samples. The method was applied to fifteen fruit samples, and low levels of pyraclostrobin and trifloxystrobin were found in two of them.