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

Els Faassen; Maria G. Antoniou; Wendy Beekman-Lukassen; Lucie Blahova; Ekaterina Chernova; Christophoros Christophoridis; Audrey Combes; Christine Edwards; Jutta Fastner; Joop Harmsen; Anastasia Hiskia; Leopold L. Ilag; Triantafyllos Kaloudis; Srdjan Lopicic; Miquel Lürling; Hanna Mazur-Marzec; Jussi Meriluoto; Cristina Porojan; Yehudit Viner-Mozzini; Nadezda Zguna

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

Els Faassen, Maria G. Antoniou, Wendy Beekman-Lukassen, Lucie Blahova, Ekaterina Chernova, Christophoros Christophoridis, Audrey Combes, Christine Edwards, Jutta Fastner, Joop Harmsen, Anastasia Hiskia, Leopold L. Ilag, Triantafyllos Kaloudis, Srdjan Lopicic, Miquel Lürling, Hanna Mazur-Marzec, Jussi Meriluoto, Cristina Porojan, Yehudit Viner-Mozzini, Nadezda Zguna

NIOO - Aquatic Ecology (AqE)

Onderzoeksoutput: Bijdrage aan wetenschappelijk tijdschrift/periodieke uitgave › Artikel › Wetenschappelijk › peer review

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Exposure to beta-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 D(3)BMAA, 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 D(3)BMAA 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.

Originele taal-2	Engels
Tijdschrift	Marine Drugs
Volume	14
Nummer van het tijdschrift	3
DOI's	https://doi.org/10.3390/md14030045
Status	Gepubliceerd - mrt. 2016

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10.3390/md14030045Licentie: CC BY

6085_Faassen
This article is an open access article distributed under the terms and conditions of the Creative Commons by Attribution (CC-BY) license (http://creativecommons.org/licenses/by/4.0/).
Final published version, 1,55 MBLicentie: CC BY

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Faassen, E., 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. (2016). A Collaborative Evaluation of LC-MS/MS Based Methods for BMAA Analysis: Soluble Bound BMAA Found to Be an Important Fraction. Marine Drugs, 14(3). https://doi.org/10.3390/md14030045

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

abstract = "Exposure to beta-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 D(3)BMAA, 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 D(3)BMAA 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.",

keywords = "6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC), seafood, phytoplankton, Daphnia magna, Liquid chromatography-tandem mass spectrometry (LC-MS/MS), beta-N-methylamino-l-alanine (BMAA), Internal standard, hydrophilic interaction liquid chromatography (HILIC), cycad, N-(2-aminoethyl) glycine (AEG), alpha,gamma-diaminobutyric acid (DAB), international",

author = "Els Faassen and Antoniou, {Maria G.} and Wendy Beekman-Lukassen and Lucie Blahova and Ekaterina Chernova and Christophoros Christophoridis and Audrey Combes and Christine Edwards and Jutta Fastner and Joop Harmsen and Anastasia Hiskia and Ilag, {Leopold L.} and Triantafyllos Kaloudis and Srdjan Lopicic and Miquel L{\"u}rling and Hanna Mazur-Marzec and Jussi Meriluoto and Cristina Porojan and Yehudit Viner-Mozzini and Nadezda Zguna",

note = "6085, AqE; Data archiving: Property of WUR",

year = "2016",

month = mar,

doi = "10.3390/md14030045",

language = "English",

volume = "14",

journal = "Marine Drugs",

issn = "1660-3397",

publisher = "Multidisciplinary Digital Publishing Institute (MDPI)",

number = "3",

}

Faassen, E, Antoniou, MG, Beekman-Lukassen, W, Blahova, L, Chernova, E, Christophoridis, C, Combes, A, Edwards, C, Fastner, J, Harmsen, J, Hiskia, A, Ilag, LL, Kaloudis, T, Lopicic, S, Lürling, M, Mazur-Marzec, H, Meriluoto, J, Porojan, C, Viner-Mozzini, Y & Zguna, N 2016, 'A Collaborative Evaluation of LC-MS/MS Based Methods for BMAA Analysis: Soluble Bound BMAA Found to Be an Important Fraction', Marine Drugs, vol. 14, nr. 3. https://doi.org/10.3390/md14030045

TY - JOUR

T1 - A Collaborative Evaluation of LC-MS/MS Based Methods for BMAA Analysis: Soluble Bound BMAA Found to Be an Important Fraction

AU - Faassen, Els

AU - Antoniou, Maria G.

AU - Beekman-Lukassen, Wendy

AU - Blahova, Lucie

AU - Chernova, Ekaterina

AU - Christophoridis, Christophoros

AU - Combes, Audrey

AU - Edwards, Christine

AU - Fastner, Jutta

AU - Harmsen, Joop

AU - Hiskia, Anastasia

AU - Ilag, Leopold L.

AU - Kaloudis, Triantafyllos

AU - Lopicic, Srdjan

AU - Lürling, Miquel

AU - Mazur-Marzec, Hanna

AU - Meriluoto, Jussi

AU - Porojan, Cristina

AU - Viner-Mozzini, Yehudit

AU - Zguna, Nadezda

N1 - 6085, AqE; Data archiving: Property of WUR

PY - 2016/3

Y1 - 2016/3

N2 - Exposure to beta-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 D(3)BMAA, 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 D(3)BMAA 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.

AB - Exposure to beta-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 D(3)BMAA, 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 D(3)BMAA 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.

KW - 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC)

KW - seafood

KW - phytoplankton

KW - Daphnia magna

KW - Liquid chromatography-tandem mass spectrometry (LC-MS/MS)

KW - beta-N-methylamino-l-alanine (BMAA)

KW - Internal standard

KW - hydrophilic interaction liquid chromatography (HILIC)

KW - cycad

KW - N-(2-aminoethyl) glycine (AEG)

KW - alpha,gamma-diaminobutyric acid (DAB)

KW - international

U2 - 10.3390/md14030045

DO - 10.3390/md14030045

M3 - Article

SN - 1660-3397

VL - 14

JO - Marine Drugs

JF - Marine Drugs

IS - 3

ER -

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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