Determination of Paralytic Shellfish Toxins and Tetrodotoxins in Shellfish by Ultra-High Performance Hydrophilic-Interaction Liquid Chromatography-Tandem Quadrupole Mass Spectrometry

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Andrew D. Turner, Mike J. Boundy, D. Tim Harwood, and Simon Hird
Waters, Cefas, Cawthron Institute
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A simple, rapid, cost-effective method for the determination of hydrophilic marine biotoxins in shellfish tissue samples is described.

The ACQUITY UPLC I-Class System with the Xevo TQ-S Mass Spectrometer provides excellent sensitivity for detection, identification, and quantification of paralytic shellfish toxins and tetrodotoxin in shellfish tissues. The method can be used for both screening and confirmation for the purpose of shellfish food safety testing. A simple single-step extraction of shellfish tissues in weak acetic acid prior to graphitized carbon solid phase extraction provided good recoveries for the compounds of interest and effective removal of co-extractives and salts, the source of significant matrix suppression during the analysis of shellfish by mass spectrometry. The Xevo TQ-S exhibited excellent sensitivity and robustness, but this same method could easily be transferred to other Xevo tandem quadrupole MS/MS instruments to meet the same performance criteria or extracts diluted further prior to UPLC-MS/MS.

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