Selective quantification of the neurotoxin BMAA by use of hydrophilic-interaction liquid chromatography–differential mobility spectrometry–tandem mass spectrometry (HILIC–DMS–MS–MS)

From National Research Council Canada

DOIResolve DOI: https://doi.org/10.1007/s00216-015-9012-8
AuthorSearch for: 1; Search for: 1; Search for: 1
Name affiliation
  1. National Research Council of Canada. Measurement Science and Standards
FormatText, Article
Journal titleAnalytical and Bioanalytical Chemistry
ISSN1618-2642
1618-2650
Abstract
The neurotoxin β-N-methylamino-l-alanine (BMAA) has been reported in cyanobacteria and shellfish, raising concerns about widespread human exposure. However, inconsistent results for BMAA analysis have led to controversy. Liquid chromatography–tandem mass spectrometry (LC–MS–MS) is the most appropriate method for analysis of BMAA, but the risk of interference from isomers, other sample components, and the electrospray background is still present. We have investigated differential mobility spectrometry (DMS) as an ion filter to improve selectivity in the hydrophilic interaction liquid chromatographic (HILIC)–MS–MS determination of BMAA. We obtained standards for two BMAA isomers not previously analyzed by HILIC–MS, β-amino-N-methylalanine and 3,4-diaminobutanoic acid, and the typically used 2,4-diaminobutanoic acid and N-(2-aminoethyl)glycine. DMS separation of BMAA from these isomers was achieved and optimized conditions were used to develop a sensitive and highly selective multidimensional HILIC–DMS–MS–MS method. This work revealed current technical limitations of DMS for trace quantification, and practical solutions were implemented. Accurate control of low levels of DMS carrier gas modifier was essential, but required external metering. The linearity of our optimized method was excellent from 0.01 to 6 μmol L−1. The instrumental LOD was 0.4 pg BMAA injected on-column and the estimated method LOD was 20 ng g−1 dry weight for BMAA in sample matrix. The method was used to analyze cycad plant tissue, a cyanobacterial reference material, and mussel tissues, by use of isotope-dilution quantification with deuterated BMAA. This confirmed the presence of BMAA and several of its isomers in cycad and mussel tissues, including commercially available mussel tissue reference materials certified for other biotoxins.
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LanguageEnglish
Peer reviewedYes
NPARC number21276018
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