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Analytical and Bioanalytical Chemistry

, Volume 407, Issue 9, pp 2473–2484 | Cite as

Analysis of paralytic shellfish toxins using high-field asymmetric waveform ion mobility spectrometry with liquid chromatography-mass spectrometry

  • Daniel G. Beach
  • Jeremy E. Melanson
  • Randy W. Purves
Research Paper

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.

Keywords

Differential mobility spectrometry (DMS) Paralytic shellfish poisoning (PSP) Algal toxins Marine biotoxins Liquid chromatography-mass spectrometry High-field asymmetric waveform ion mobility spectrometry (FAIMS) 

Notes

Acknowledgments

The authors gratefully acknowledge the technical assistance of Krista Thomas and Margaret McCooeye as well as the support and editorial assistance of Pearse McCarron and Michael Quilliam. The authors would like to thank Thermo Fisher for the loan of the TSQ Quantum.

Supplementary material

216_2015_8488_MOESM1_ESM.pdf (156 kb)
ESM 1 (PDF 156 kb)

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Copyright information

© Her Majesty the Queen in Right of Canada as represented by: National Research Council Canada 2015

Authors and Affiliations

  • Daniel G. Beach
    • 1
  • Jeremy E. Melanson
    • 2
  • Randy W. Purves
    • 3
  1. 1.Measurement Science and StandardsNational Research Council CanadaHalifaxCanada
  2. 2.Measurement Science and StandardsNational Research Council CanadaOttawaCanada
  3. 3.Plant Sciences DepartmentUniversity of SaskatchewanSaskatoonCanada

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