Liquid chromatography/negative electrospray ionization ion trap MS2 mass spectrometry application for the determination of microcystins occurrence in Southern Portugal water reservoirs

Rodrigues, Maria Aurineide; Reis, Margarida; Mateus, M.C.

doi:10.1016/j.toxicon.2013.07.013

Cited by 20 publications

(10 citation statements)

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“…Negative ionization mode by MALDI and ESI presented low absolute intensities but also low background and therefore provided suitable S/N ratios. According to other authors [19][20][21]44], as shown Table S1 of supplementary data, the analysis of MCs containing no Arg residue such as MC-LA, -LF, -LW and -LY presented high sensitivity in negative ionization mode.…”

Section: Throughput Analysis (Direct Maldi and Esi Analysis)mentioning

confidence: 81%

“…The main fragment ions of MC-LR have been included in Table 2. These fragment ions have been already described in the literature [19,21,52] but in the present manuscript all the fragment ions have been evaluated for confirmatory purposes. As shown in Fig.…”

Section: Tablementioning

confidence: 99%

“…Typically, the positive ionization mode is the most usually ionization mode employed. Additionally, electrospray (ESI) recorded in negative ion mode has recently been applied to the analysis of MCs [19][20][21]. In order to have faster methods for toxin analysis: ultra-high performance liquid chromatography (UHPLC) [22][23][24], on-line solid phase extraction (SPE) [25][26][27][28] and direct analysis without prior extraction [29,30] and chromatographic separation [31,32] have been implemented in several works.…”

Section: Introductionmentioning

confidence: 99%

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An integrated strategy for rapid and accurate determination of free and cell-bound microcystins and related peptides in natural blooms by liquid chromatography–electrospray-high resolution mass spectrometry and matrix-assisted laser desorption/ionization time-of-flight/time-of-flight mass spectrometry using both positive and negative ionization modes

Flores

Caixach

2015

Journal of Chromatography A

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An integrated high resolution mass spectrometry (HRMS) strategy has been developed for rapid and accurate determination of free and cell-bound microcystins (MCs) and related peptides in water blooms. The natural samples (water and algae) were filtered for independent analysis of aqueous and sestonic fractions. These fractions were analyzed by MALDI-TOF/TOF-MS and ESI-Orbitrap-HCD-MS. MALDI, ESI and the study of fragmentation sequences have been provided crucial structural information. The potential of combined positive and negative ionization modes, full scan and fragmentation acquisition modes (TOF/TOF and HCD) by HRMS and high resolution and accurate mass was investigated in order to allow unequivocal determination of MCs. Besides, a reliable quantitation has been possible by HRMS. This composition helped to decrease the probability of false positives and negatives, as alternative to commonly used LC-ESI-MS/MS methods. The analysis was non-target, therefore covered the possibility to analyze all MC analogs concurrently without any pre-selection of target MC. Furthermore, archived data was subjected to retrospective "post-targeted" analysis and a screening of other potential toxins and related peptides as anabaenopeptins in the samples was done. Finally, the MS protocol and identification tools suggested were applied to the analysis of characteristic water blooms from Spanish reservoirs.

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Section: Throughput Analysis (Direct Maldi and Esi Analysis)mentioning

confidence: 81%

Section: Tablementioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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An integrated strategy for rapid and accurate determination of free and cell-bound microcystins and related peptides in natural blooms by liquid chromatography–electrospray-high resolution mass spectrometry and matrix-assisted laser desorption/ionization time-of-flight/time-of-flight mass spectrometry using both positive and negative ionization modes

Flores

Caixach

2015

Journal of Chromatography A

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“…Tandem mass spectrometry (MS/MS) has been widely adopted for the routine quantitative analyses of target cyanotoxins in water samples using the very sensitive multiple reaction monitoring (MRM) mode of triple quadrupole (QqQ) mass spectrometers [23,[25][26][27][28][29][30][31]. For structural characterization and quantitation purposes, 3D ion trap (IT) [32][33][34][35][36][37], linear ion trap (LIT) [38], time-of-flight (TOF) [39,40], Q-TOF [41][42][43][44][45] and Orbitrap mass spectrometers [26,[46][47][48][49][50][51][52] were employed. High mass accuracy of TOF and Orbitrap instruments is beneficial for LC-MS and LC-MS/MS analyses of cyanotoxins [24].…”

Section: Introductionmentioning

confidence: 99%

High Levels of Anabaenopeptins Detected in a Cyanobacteria Bloom from N.E. Spanish Sau-Susqueda-El Pasteral Reservoirs System by LC–HRMS

Flores

Caixach

2020

Toxins

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The appearance of a bloom of cyanobacteria in the Sau-Susqueda-El Pasteral system (River Ter, NE Spain) in the autumn of 2015 has been the most recent episode of extensive bloom detected in Catalonia. This system is devoted mainly to urban supply, regulation of the river, irrigation and production of hydroelectric energy. In fact, it is one of the main supply systems for the metropolitan area of cities such as Barcelona and Girona. An assessment and management plan was implemented in order to minimize the risk associated to cyanobacteria. The reservoir was confined and periodic sampling was carried out. Low and high toxicity was detected by cell bioassays with human cell lines. Additionally, analysis studies were performed by enzyme-linked immunosorbent assay (ELISA) and liquid chromatography–high resolution mass spectrometry (LC–HRMS). A microcystin target analysis and suspect screening of microcystins, nodularins, cylindrosperpmopsin and related cyanobacterial peptides by LC–HRMS were applied. The results for the analysis of microcystins were negative (<0.3 μg/L) in all the surface samples. Only traces of microcystin-LR, -RR and -dmRR were detected by LC–HRMS in a few ng/L from both fractions, aqueous and sestonic. In contrast, different anabaenopeptins and oscillamide Y at unusually high concentrations (µg-mg/L) were observed. To our knowledge, no previous studies have detected these bioactive peptides at such high levels. The reliable identification of these cyanobacterial peptides was achieved by HRMS. Although recently these peptides are detected frequently worldwide, these bioactive compounds have received little attention. Therefore, more studies on these substances are recommended, especially on their toxicity, health risk and presence in water resources.

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“…Sendo assim, um espectrômetro de massas consiste em uma fonte de ionizaçaõ para a obtençaõ de ións, um analisador de massas, o qual separa os ións formados, um detector desses ións e um sistema de aquisiçaõ dos dados(CAIXACH et al, 2017). outras moléculas como uma abordagem padrão para fins quantitativos, embora o ESI modo negativo também tenha sido usado para análise de certas cianotoxinasGAMBARO et al, 2012;RODRIGUES;REIS;MATEUS, 2013). Nodularia spumigena CENA596 encontrada no oceano Atlântico Sul do Brasil apresenta diversidade de agrupamentos gênicos envolvidos na síntese de moléculas bioativas e diferenças significativas quando comparado com o único genoma disponível dessa espécie, a Nodularia spumigena CCY9414 originária do mar Báltico.A redução de bactérias contaminantes na cultura da N. spumigena CENA596 foi feita conforme a metodologia apresentada porVaz et al (2014).…”

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Análise genômica e funcional da Nodularia spumigena CENA596 formadora de florações em tanques de produção de camarões

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Liquid chromatography/negative electrospray ionization ion trap MS2 mass spectrometry application for the determination of microcystins occurrence in Southern Portugal water reservoirs

Cited by 20 publications

References 42 publications

High Levels of Anabaenopeptins Detected in a Cyanobacteria Bloom from N.E. Spanish Sau-Susqueda-El Pasteral Reservoirs System by LC–HRMS

Análise genômica e funcional da Nodularia spumigena CENA596 formadora de florações em tanques de produção de camarões

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