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Mar. Drugs 2016, 14(3), 45; doi:10.3390/md14030045

A Collaborative Evaluation of LC-MS/MS Based Methods for BMAA Analysis: Soluble Bound BMAA Found to Be an Important Fraction

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Aquatic Ecology & Water Quality Management Group, Wageningen University, P.O. Box 47, Wageningen 6700 DD, The Netherlands
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Department of Environmental Science and Technology, Cyprus University of Technology, 3036 Lemesos, Cyprus
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Faculty of Science, RECETOX, Masaryk University, Kamenice 5, 625 00 Brno, Czech Republic
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Saint-Petersburg Scientific-Research Centre for Ecological Safety, Russian Academy of Sciences, 18, Korpusnaya street, St. Petersburg 197110, Russia
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Laboratory of Catalytic—Photocatalytic Processes and Environmental Analysis, Institute of Nanoscience & Nanotechnology, National Center for Scientific Research “Demokritos”, Patriarchou Grigoriou & Neapoleos, 15310 Agia Paraskevi, Athens, Greece
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Department of Analytical, Bioanalytical Sciences and Miniaturization (LSABM), UMR CBI 8231 ESPCI ParisTech/CNRS, PSL Research University, ESPCI ParisTech, 75005 Paris, France
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Pharmacy & Life Sciences, Robert Gordon University, Aberdeen AB10 7GJ, UK
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Drinking-Water Resources and Water Treatment, Federal Environment Agency, Schichauweg 58, 12307 Berlin, Germany
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Alterra, P.O. Box 47, Wageningen 6700 DD, The Netherlands
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Department of Environmental Science and Analytical Chemistry, Stockholm University, SE-10691 Stockholm, Sweden
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Water Quality Department, Division of Quality, Research and Development (R&D), Athens Water Supply and Sewerage Company (EYDAP SA), 156 Oropou str., 11146 Athens, Greece
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Institute for Pathological Physiology, School of Medicine, University of Belgrade, 11000 Belgrade, Serbia
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NIOO-KNAW, Droevendaalsesteeg 10, Wageningen 6708 PB, The Netherlands
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Department of Marine Biotechnology, University of Gdansk, Al. Marszalka Pilsudskiego 46, Gdynia 81-378, Poland
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Biochemistry, Faculty of Science and Engineering, Åbo Akademi University, Tykistökatu 6A 3rd Floor, Turku 20520, Finland
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Mass Spectrometry Research Centre (MSRC) and PROTEOBIO Research Groups, Department of Physical Sciences, Cork Institute of Technology, Rossa Avenue, Bishopstown, V92 F9WY, Co. Cork, Ireland
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Kinneret Limnological Laboratory, Israel Oceanographic & Limnological Research, P.O. Box 447, Migdal 14950, Israel
*
Author to whom correspondence should be addressed.
Academic Editors: Lucio G. Costa and Vítor Vasconcelos
Received: 15 October 2015 / Revised: 26 January 2016 / Accepted: 6 February 2016 / Published: 29 February 2016
(This article belongs to the Special Issue Marine Neurotoxins)
View Full-Text   |   Download PDF [1587 KB, uploaded 29 February 2016]   |  

Abstract

Exposure to β-N-methylamino-l-alanine (BMAA) might be linked to the incidence of amyotrophic lateral sclerosis, Alzheimer’s disease and Parkinson’s disease. Analytical chemistry plays a crucial role in determining human BMAA exposure and the associated health risk, but the performance of various analytical methods currently employed is rarely compared. A CYANOCOST initiated workshop was organized aimed at training scientists in BMAA analysis, creating mutual understanding and paving the way towards interlaboratory comparison exercises. During this workshop, we tested different methods (extraction followed by derivatization and liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) analysis, or directly followed by LC-MS/MS analysis) for trueness and intermediate precision. We adapted three workup methods for the underivatized analysis of animal, brain and cyanobacterial samples. Based on recovery of the internal standard D3BMAA, the underivatized methods were accurate (mean recovery 80%) and precise (mean relative standard deviation 10%), except for the cyanobacterium Leptolyngbya. However, total BMAA concentrations in the positive controls (cycad seeds) showed higher variation (relative standard deviation 21%–32%), implying that D3BMAA was not a good indicator for the release of BMAA from bound forms. Significant losses occurred during workup for the derivatized method, resulting in low recovery (<10%). Most BMAA was found in a trichloroacetic acid soluble, bound form and we recommend including this fraction during analysis. View Full-Text
Keywords: β-N-methylamino-l-alanine (BMAA); 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC); α,γ-diaminobutyric acid (DAB); cycad; Daphnia magna; hydrophilic interaction liquid chromatography (HILIC); Internal standard; Liquid chromatography-tandem mass spectrometry (LC-MS/MS); N-(2-aminoethyl) glycine (AEG); phytoplankton; seafood β-N-methylamino-l-alanine (BMAA); 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC); α,γ-diaminobutyric acid (DAB); cycad; Daphnia magna; hydrophilic interaction liquid chromatography (HILIC); Internal standard; Liquid chromatography-tandem mass spectrometry (LC-MS/MS); N-(2-aminoethyl) glycine (AEG); phytoplankton; seafood
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MDPI and ACS Style

Faassen, E.J.; Antoniou, M.G.; Beekman-Lukassen, W.; Blahova, L.; Chernova, E.; Christophoridis, C.; Combes, A.; Edwards, C.; Fastner, J.; Harmsen, J.; Hiskia, A.; Ilag, L.L.; Kaloudis, T.; Lopicic, S.; Lürling, M.; Mazur-Marzec, H.; Meriluoto, J.; Porojan, C.; Viner-Mozzini, Y.; Zguna, N. A Collaborative Evaluation of LC-MS/MS Based Methods for BMAA Analysis: Soluble Bound BMAA Found to Be an Important Fraction. Mar. Drugs 2016, 14, 45.

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