The analysis of biological toxins from aquatic sources (i.e. both marine and freshwater) has been an active area of research for many years. These toxins are typically secondary metabolites produced by algal or cyanobacterial sources and involved with food and water poisoning. These include toxins such as saxitoxin, tetrodotoxin, brevetoxin, palytoxin and many others. The majority of methods applied to toxin detection have been based on either enzyme-linked immunosorbent assays (ELISAs) when available or high performance liquid chromatography coupled to mass spectrometry (HPLC-MS). HPLC-MS methods are more universally used for toxin detection and are often based on hydrophilic interaction liquid chromatography (HILIC) for the hydrophilic toxins or reverse phase (RP) liquid chromatography for hydrophobic toxins. While many of these methods are sensitive, accurate, and quantitative, they are typically targeted to a single toxin or small class of toxins. This is mirrored by the extraction techniques employed prior to detection, which also use a specific solvent based on analyte/toxin characteristics. . When the identity of the toxin is unknown, techniques for screening a broader collection of toxins are needed. This is particularly true for forensic applications.  <br/>We have applied a combined method for comprehensive toxin extraction along with a tandem HPLC approach to detect a wide variety of aquatic toxins. The goal of this method is to partition hydrophobic and hydrophilic metabolites into different liquid phases that can be analyzed separately. The liquid-liquid extraction used in this work builds on methods for extraction of metabolites and proteins from environmental samples. The tandem HPLC-MS approach utilizes both HILIC and RP modes of separation to profile a collection of toxins ranging from hydrophilic tetrodotoxin to hydrophobic ciguatoxin. This tandem HPLC approach has been applied to both single solvent extractions as well as combined liquid-liquid extractions of samples. The extraction and analysis method has been applied to aquatic samples (e.g. fish) to determine the effectiveness of the method in the presence of complex matrices.<br/>

Comprehensive analysis of aquatic toxins by HPLC-MS/MS

253rd National Meeting (2017)

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