Simultaneous determination of twelve paralytic shellfish poisoning toxins in bivalve molluscs by UPLC-MS/MS and its applications to a food poisoning incident

In this study, an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was originally developed for simultaneously quantitative analysis of twelve paralytic shellfish poisoning toxins, referring to STX, NEO, dcSTX, GTX1, GTX2, GTX3, GTX4, GTX5, C1, C2, dcGTX2, and dcGTX3 in bivalve molluscs. Chromatographic separations were performed on a TSK-Gel Amide-80 column (5 μm, 2.0 × 150 mm, Tosoh Corporation) by gradient elution with 2 mmol L^-1 ammonium formate solution-acetonitrile (containing 0.1% formic acid) as mobile phases. The samples were pretreated by extraction with acetonitrile-water (80:20, v/v; containing 0.1% formic acid), followed by cleaning up using an Oasis HLB extraction cartridge (500 mg/6 mL). The present method showed good linearity (r² > 0.99) with the limits of detection (LODs) and limits of quantification (LOQs) ranged from 1.03 to 10.65 μg/kg and 3.43-35.46 μg/kg, respectively for these toxins. Owing to its sensitivity and rapid properties, the presented method was applied to the determination of PSP toxins in bivalve molluscs involved in a food poisoning incident occurred in Zhangzhou, China, in June 2017.