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. 2023 Dec 7;36(12):1834–1863. doi: 10.1021/acs.chemrestox.3c00241

Table 5. Detection of Bacterial and Marine Biotoxins by MS-Based Approach.

Name Sample Method Operating parameters Outcome Ref
Enterotoxin Commercial LC–HRMS LC–MS Q-extractive mass spectrophotometer C18 reverse phase column; isocratic elution 93 signature peptides identified for enterotoxins (182)
Botulinum Commercial Endopep MS Triple quadrupole mass spectrometer; Turbo Ion Spray interface; C18 column; gradient elution Toxin detection 0.1 MLD50 and quantification 0.62 MLD50 (183)
Okadaic acid Raw and cooked food (Mussel, clam, flatfish) Tandem mass spectrometry C18 column with triple-quadruple mass spectrometer; ammonium format gradient elution; negative ionization mode LOD and accuracy 0.2–5.1 μg/k (184)
Dinophysistoxin Raw and cooked food (Mussel, clam, flatfish) Tandem mass spectrometry C18 column with triple-quadruple mass spectrometer; ammonium format gradient elution; negative ionization mode LOD and accuracy 0.2–5.1 μg/k (184)
Anatoxins a (ATX) and Homoanatoxin-a (HAT) Benthic-cyanobacterial-mat field samples LC–HRMS/MS Q Exactive HF Orbitrap MS; HESI-II electrospray ionization source; at 40 °C; resolution 60,000; collision energy 20 eV Toxins are in conjugated form 15% ATX and 38% HAT (185)
Cyanotoxins Blue-green algae dietary supplement Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry Electrospray ionization positive; source temperature 550 °C; ion spray voltage 5500 V; curtain gas 25 psi; collision gas 10 psi Quantification limits 60–300 μg kg–1 (186)
Paralytic shellfish toxins Marine shellfish Hydrophilic interaction chromatography-tandem mass spectrometry Separation with HILIC-Z column; acetonitrile and ammonium formate-formic acid as the mobile phase; positive electrospray ionization; samples are cleaned with by ion-pair SPE using a porous graphitic carbon cartridge Limits of detection 1.7–13.7 μg kg–1; and quantitation 5.2–41.0 μg kg–1; recoveries 76.5–95.5% (187)
Tetrodotoxin Marine shellfish Hydrophilic interaction chromatography-tandem mass spectrometry Separation with HILIC-Z column; acetonitrile and ammonium formate-formic acid as the mobile phase; positive electrospray ionization; samples are cleaned with by ion-pair SPE using a porous graphitic carbon cartridge Limits of detection 1.7–13.7 μg kg–1; and quantitation 5.2–41.0 μg kg–1; recoveries 76.5–95.5%