Determination of hydrophilic marine biotoxins in bivalve molluscs by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS)

This work describes a method for the determination of paralytic shellfish toxins in mussels (M. galloprovincialis), oysters (Crassostrea gigas), and clams (Ruditapes decussatus) samples. The acetic acid extraction method is used for simultaneous analysis of Paralytic Shellfish Poisoning (PSP) and the separation of these compounds was achieved on ethylene bridged hybrid (BEH) Amide column with gradient mobile phase composed of acetonitrile (MeCN) and water (as eluent A and eluent B) both containing 2mM ammonium formate and 50mM formic acid. The method specificity, linearity, sensitivity, precision, and accuracy were successfully evaluated towards the detection of 13 hydrophilic marine biotoxins analyzed together (single run) indifferent sample matrixes such as mussels. oysters. and clams. Calibration curves were found to be linear (R2 ≥ 0.99). average Recovery% of 98.5–99.9%. limits of detection (LODs): 0.16–1.92µg·kg−1; limits of quantitation (LOQs): 0.54–6.41µg·kg−1) and the relative standard deviation (RSD%) of the precision was ≤ 2.8%. The method was applied for the determination of PSP in shellfish collected from several Tunisian locations. All LC-MS/MS results of analyzed molluscs collected from different Tunisia locations, reveal no PSP toxin group contamination and that the amount found does not exceeding the threshold of 800µg STXequ·kg−1.