title: Analysis of paralytic shellfish toxins using high-field asymmetric waveform ion mobility spectrometry with liquid chromatography-mass spectrometry.
abstract: The analysis of paralytic shellfish toxins (PSTs) by liquid chromatography-mass spectrometry remains a challenge because of their high polarity, large number of analogues and the complex matrix in which they occur. Here we investigate the potential utility of high-field asymmetric waveform ion mobility spectrometry (FAIMS) as a gas-phase ion separation tool for analysis of PSTs by mass spectrometry. We investigate the separation of PSTs using FAIMS with two divergent goals: using FAIMS as a primary separation tool for rapid screening by electrospray ionization (ESI)-FAIMS-MS or combined with LC in a multidimensional LC-ESI-FAIMS-MS separation. First, a survey of the parameters that affect the sensitivity and selectivity of PST analysis by FAIMS was carried out using ESI-FAIMS-MS. In particular, the use of acetonitrile as a gas additive in the carrier gas flow offered good separation of all PST epimeric pairs. A second set of FAIMS conditions was also identified, which focussed PSTs to a relatively narrow CV range allowing development of an LC-ESI-FAIMS-MS method for analysis of PST toxins in complex mussel tissue extracts. The quantitative capabilities of this method were evaluated by analysing a PST containing mussel tissue matrix material. Results compared favourably with analysis by an established LC-post-column oxidation-fluorescence method with recoveries ranging from 70 to 106%, although sensitivity was somewhat reduced. The current work represents the first successful separation of PST isomers using ion mobility and shows the promise of FAIMS as a tool for analysis of algal biotoxins in complex samples and outlines some critical requirements for its future improvement.
authors.affiliation: Measurement Science and Standards, National Research Council Canada, Halifax, NS, B3H 3Z1, Canada, daniel.beach@nrc-cnrc.gc.ca.
authors.forename: Daniel G
authors.initials: DG
authors.lastname: Beach
authors.forename: Jeremy E
authors.initials: JE
authors.lastname: Melanson
authors.forename: Randy W
authors.initials: RW
authors.lastname: Purves
mesh_terms: D000818:Animals; D049872:Bivalvia / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D008387:Marine Toxins / Q000737:chemistry* / Q000633:toxicity; D013058:Mass Spectrometry / Q000379:methods*; D015394:Molecular Structure; D012758:Shellfish / Q000032:analysis*
chemical_list: D008387:Marine Toxins