Four Paralytic Shellfish Poisonings Determination in Aquatic Products by UPLC-MS/MS Spectrometry

Objectives To develop an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the determination of four paralytic shellfish poisonings (PSP) in aquatic products.

Methods Samples were ultrasonically extracted by 0.1mol/L acetic acid, then purified by OASIS HLB solid phase extraction (SPE). Four PSPs were separated by HILIC with mobile phase of acetonitrile and ammonium acetate in 0.1% formic acid. Analytic identification and quantification were performed by electrospray ionization (ESI) in positive mode using multiple reaction monitoring (MRM). Quantification was performed by external standard.

Results Four paralytic shellfish poisonings could be separated well from impurities. There was a good linearity in the range of respective working concentration, with a correlation coefficient > 0.999. The limit of quantification was in the range of 10.0 μg/kg~31.0 μg/kg for four PSPs; the average recoveries at different concentration were 81.0%~104% (n = 6), and the relative standard deviations were 0.47%~6.9%.

Conclusions This method was simple, sensitive and repeatable, which was suitable for the confirmation and quantitative analysis of PSP in shellfish.