Determination of the non protein amino acid β-N-methylamino-l-alanine in estuarine cyanobacteria by capillary electrophoresis

Baptista, Mafalda S.; Cianca, Rosa Carmina Cervantes; Lopes, Viviana R.; Almeida, C. Marisa R.; Vasconcelos, Vı́tor

doi:10.1016/j.toxicon.2011.08.007

Cited by 29 publications

(20 citation statements)

References 29 publications

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“…In contrast, all but one [121] later studies could not reproduce these first results; BMAA was either not detected in cyanobacteria (e.g. [76,77]), detected in some, yet not all, samples [102] or detected in all samples, but at very low concentrations [83].…”

Section: Introductionmentioning

confidence: 81%

“…More work is for instance needed to explain the differences in concentrations found in cyanobacterial field isolates from similar regions and grown under similar condition that were analysed by the same group by GC-MS and LC-MS [36,122]. Also the high concentrations found by CE analysis [121] are interesting, even though the authors of this last manuscript acknowledge that the selectivity of their method is low. In general, comparison of the quantitative results of different studies is hampered by the absence of recovery and validation data in many publications.…”

Section: Discussionmentioning

confidence: 97%

“…For sixteen methods, most data needed for method validation (detection limits, linear range, precision and recovery) were provided [34,76,79,82,93,94,100,105,111,121,122,135,145,148]. However, unvalidated methods (or methods for which no sufficient validation data were provided) were repeatedly referred to as 'validated'.…”

Section: Methods Performancementioning

confidence: 99%

“…[82,95,144,147,157,159,163]). Especially in studies in which optical detection was used as the primary analytical method and in which high BMAA concentrations were found using these methods [96,121,133,144]; no reference to the debate on concentrations and methods was made.…”

Section: Selective Use Of Referencesmentioning

confidence: 99%

“…The detection of BMAA in the cyanobacterium Nostoc sp. that lives in symbiosis with the cycads [32] prompted the screening of cyanobacteria from all over the world for BMAA [33,35,36,76,77,83,94,102,107,111,[120][121][122].…”

Section: Introductionmentioning

confidence: 99%

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The neurotoxin BMAA in aquatic systems : analysis, occurrence and effects

Faassen

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Section: Introductionmentioning

confidence: 81%

Section: Discussionmentioning

confidence: 97%

Section: Methods Performancementioning

confidence: 99%

Section: Selective Use Of Referencesmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

The neurotoxin BMAA in aquatic systems : analysis, occurrence and effects

Faassen

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Determination of BMAA and three alkaloid cyanotoxins in lake water using dansyl chloride derivatization and high-resolution mass spectrometry

2015

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A new analytical method was developed for the detection of alkaloid cyanotoxins in harmful algal blooms. The detection of the nonproteinogenic amino acid β-N-methylamino-L-alanine (BMAA) and two of its conformation isomers, 2,4-diaminobutyric acid (DAB) and N-(2-aminoethyl) glycine (AEG), as well as three alkaloid cyanotoxins, anatoxin-a (ANA-a), cylindrospermopsin (CYN), and saxitoxin (STX), is presented. The use of a chemical derivatization with dansyl chloride (DNS) allows easier separation with reversed phase liquid chromatography. Detection with high-resolution mass spectrometry (HRMS) with the Q-Exactive enables high selectivity with specific fragmentation as well as exact mass detection, reducing considerably the possibilities of isobaric interferences. Previous to analysis, a solid phase extraction (SPE) step is used for purification and preconcentration. After DNS derivatization, samples are submitted to ultra high-performance liquid chromatography coupled with heated electrospray ionisation and the Q-Exactive mass spectrometer (UHPLC-HESI-HRMS). With an internal calibration using isotopically-labeled DAB-D3, the method was validated with good linearity (R (2) > 0.998), and method limits of detection and quantification (MLD and MLQ) for target compounds ranged from 0.007 to 0.01 μg L(-1) and from 0.02 to 0.04 μg L(-1), respectively. Accuracy and within-day/between-days variation coefficients were below 15%. SPE recovery values ranged between 86 and 103%, and matrix effects recovery values ranged between 75 and 96%. The developed analytical method was successfully validated with 12 different lakes samples, and concentrations were found ranging between 0.009 and 0.3 μg L(-1) except for STX which was not found in any sample.

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Quantitative determination of the neurotoxin β-N-methylamino-l-alanine (BMAA) by capillary electrophoresis–tandem mass spectrometry

2016

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Recent reports of the widespread occurrence of the neurotoxin β-N-methylamino-L-alanine (BMAA) in cyanobacteria and particularly seafood have raised concerns for public health. LC-MS/MS is currently the analytical method of choice for BMAA determinations but incomplete separation of isomeric and isobaric compounds, matrix suppression and conjugated forms are plausible limitations. In this study, capillary electrophoresis (CE) coupled with MS/MS has been developed as an alternative method for the quantitative determination of free BMAA. Using a bare fused silica capillary, a phosphate buffer (250 mM, pH 3.0) and UV detection, it was possible to separate BMAA from four isomers, but the limit of detection (LOD) of 0.25 μg mL proved insufficient for analysis of typical samples. Coupling the CE to a triple quadrupole MS was accomplished using a custom sheath-flow interface. The best separation was achieved with a 5 M formic acid in water/acetonitrile (9:1) background electrolyte. Strong acid hydrolysis of lyophilized samples was used to release BMAA from conjugated forms. Field-amplified stacking after injection was achieved by lowering sample ionic strength with a cation-exchange cleanup procedure. Quantitation was accomplished using isotope dilution with deuterium-labelled BMAA as internal standard. An LOD for BMAA in solution of 0.8 ng mL was attained, which was equivalent to 16 ng g dry mass in samples using the specified extraction procedure. This was comparable with LC-MS/MS methods. The method displayed excellent resolution of amino acid isomers and had no interference from matrix components. The presence of BMAA in cycad, mussel and lobster samples was confirmed by CE-MS/MS, but not in an in-house cyanobacterial reference material, with quantitative results agreeing with those from LC-MS/MS. Graphical Abstract CE-MS separation and detection of BMAA, its isomers and the internal standard BMAA-d3.

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Determination of the non protein amino acid β-N-methylamino-l-alanine in estuarine cyanobacteria by capillary electrophoresis

Cited by 29 publications

References 29 publications

The neurotoxin BMAA in aquatic systems : analysis, occurrence and effects

The neurotoxin BMAA in aquatic systems : analysis, occurrence and effects

Determination of BMAA and three alkaloid cyanotoxins in lake water using dansyl chloride derivatization and high-resolution mass spectrometry

Quantitative determination of the neurotoxin β-N-methylamino-l-alanine (BMAA) by capillary electrophoresis–tandem mass spectrometry

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