On-line solid-phase extraction coupled to liquid chromatography tandem mass spectrometry for the analysis of cyanotoxins in algal blooms

Fayad, Paul B.; Roy-Lachapelle, Audrey; Duy, Sung Vo; Prévost, Michèle; Sauvé, Sébastien

doi:10.1016/j.toxicon.2015.10.010

Cited by 51 publications

(35 citation statements)

References 41 publications

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“…For the analysis of ANA-a via the LDTD-APCI-HRMS method and of MCs and ANA-a via the UHPLC-HESI-HRMS system, the weighed samples were mixed with 5 mL of acidified MeOH (formic acid, pH 2) in polyethylene conical-bottom centrifuge tubes [27,31]. The samples were homogenized for 10 min using ultrasonication and then they were submitted to centrifugation at 3500 rpm for 10 min.…”

Section: Methodsmentioning

confidence: 99%

“…The chromatographic column was a Hypersil GOLD TM C18 column (100 mm, 2.1 mm, 1.9 µm particles) preceded by a guard column (5 mm, 2.1 mm, 3 µm particles) (Thermo Fisher Scientific, Waltham, MA, USA). Chromatographic settings are presented in Table 4 for both analytical methods and are based on published optimization parameters [31,33]. For the analysis of MCs and ANA-a, the injection volume was 25 µL and flow rate was set at 525 µL∙min −1 with a constant temperature of 55 °C.…”

Section: Methodsmentioning

confidence: 99%

“…More specifically, Lemieux oxidation using potassium permanganate and sodium periodate allowed the recovery of the 2-methyl-3-methoxy-4-phenylbutyric acid (MMPB) moiety common to all MCs which includes over 100 known congeners [30]. Samples were also submitted to ultra-high performance liquid chromatography-heated electrospray (UHPLC-HESI) coupled to HRMS, which were previously developed and ultimately adapted for this project [31]. The MC congeners present in the samples were then identified and quantified and results were compared with total MCs quantification results.…”

Section: Introductionmentioning

confidence: 99%

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Detection of Cyanotoxins in Algae Dietary Supplements

Roy-Lachapelle

Solliec

Bouchard

et al. 2017

Toxins

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105

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Algae dietary supplements are marketed worldwide as natural health products. Although their proprieties have been claimed as beneficial to improve overall health, there have been several previous reports of contamination by cyanotoxins. These products generally contain non-toxic cyanobacteria, but the methods of cultivation in natural waters without appropriate quality controls allow contamination by toxin producer species present in the natural environment. In this study, we investigated the presence of total microcystins, seven individual microcystins (RR, YR, LR, LA, LY, LW, LF), anatoxin-a, dihydroanatoxin-a, epoxyanatoxin-a, cylindrospermopsin, saxitoxin, and β-methylamino-l-alanine in 18 different commercially available products containing Spirulina or Aphanizomenon flos-aquae. Total microcystins analysis was accomplished using a Lemieux oxidation and a chemical derivatization using dansyl chloride was needed for the simultaneous analysis of cylindrospermopsin, saxitoxin, and β-methylamino-l-alanine. Moreover, the use of laser diode thermal desorption (LDTD) and ultra-high performance liquid chromatography (UHPLC) both coupled to high resolution mass spectrometry (HRMS) enabled high performance detection and quantitation. Out of the 18 products analyzed, 8 contained some cyanotoxins at levels exceeding the tolerable daily intake values. The presence of cyanotoxins in these algal dietary supplements reinforces the need for a better quality control as well as consumer’s awareness on the potential risks associated with the consumption of these supplements.

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Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Detection of Cyanotoxins in Algae Dietary Supplements

Roy-Lachapelle

Solliec

Bouchard

et al. 2017

Toxins

Self Cite

105

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“…All 12 standards had a purity over 95%, and in each case 10 ppm in methanol was prepared as identification references. The oligopeptide nodularin has been used in previous studies as an internal standard to estimate the recovery of microcystins during extraction [32,65,66]. It has not been found to date in freshwater cyanobacteria or freshwater environmental samples and appears restricted to the marine environment.…”

Section: Extractionmentioning

confidence: 99%

“…Untargeted metabolomics (also referred to as nontarget analysis) studies the overall change of the metabolome without targeting specific compounds; it is a qualitative analysis that facilitates the detection of metabolites without prior knowledge of their presence, as well as potentially novel compounds [30]. Cyanobacteria metabolites have been studied by applying both targeted and untargeted metabolomics approaches with a major focus on microcystins [31][32][33][34][35][36][37][38][39][40] while targeted metabolomics have most commonly been applied to enable the identification of a few less studied metabolites (e.g., aeruginosins, β-methylamino-L-alanine, cyanobactins) [41][42][43][44]. This latter approach is useful but does not represent the entire diversity of metabolites at the metabolome level.…”

Section: Introductionmentioning

confidence: 99%

Metabolome Variation between Strains of Microcystis aeruginosa by Untargeted Mass Spectrometry

Racine

Saleem

Pick

2019

Toxins

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Cyanobacteria are notorious for their potential to produce hepatotoxic microcystins (MCs), but other bioactive compounds synthesized in the cells could be as toxic, and thus present interest for characterization. Ultra performance liquid chromatography and high-resolution accurate mass spectrometry (UPLC-QTOF-MS/MS) combined with untargeted analysis was used to compare the metabolomes of five different strains of the common bloom-forming cyanobacterium, Microcystis aeruginosa. Even in microcystin-producing strains, other classes of oligopeptides including cyanopeptolins, aeruginosins, and aerucyclamides, were often the more dominant compounds. The distinct and large variation between strains of the same widespread species highlights the need to characterize the metabolome of a larger number of cyanobacteria, especially as several metabolites other than microcystins can affect ecological and human health.Key Contribution: Metabolome variation between M. aeruginosa strains, highlighted by oligopeptide detection and identification, using a new, untargeted analytical workflow.Toxins 2019, 11, 723 2 of 18 and Planktothrix [17,18], MCs cause the inhibition of protein phosphatases 2A and 1 in vertebrates, which leads to an accumulation of phosphorylated proteins in cells. This accumulation can affect different metabolic pathways, including the inhibition of tumor suppressor proteins, cell proliferation and eventually, death [9,[19][20][21]. Despite many ecological impacts, the biological role of MCs within cyanobacteria remains unknown, which makes their control difficult. Remarkably, the cell concentrations of MCs in toxigenic taxa can reach those of chlorophyll a [22], the primary pigment involved in photosynthesis in cyanobacteria, algae and higher plants.Thus far over 269 variants have been identified with molecular weights varying between 880 and 1200 Da [10,23]. Amino acid variation in various positions of the cyclic molecule affects the degree of toxicity in vertebrates, as shown by LD 50 values between 50 µg/kg (MC-LA) and 800 µg/kg (MC-RR) in mice after intraperitoneal injection [16]. Microcystins are thus potentially more lethal to vertebrates than several highly potent poisons, such as sarin [24]. Increasing toxic effects are observed when hydrophobic amino acids (e.g., methylated amino acids) are present in the molecule, which can facilitate MC penetration into the tissues [25]. However, the ADDA moiety of the molecule (3-amino-9-methoxy-10-phenyl-2,6,8-trimethyldeca-4,6-dienoic acid), found in all MC variants, is known to have a major role in the toxicity [25].In addition to microcystins, cyanobacteria can produce a wide range of bioactive compounds. These include an extraordinary diversity of oligopeptides (e.g., cyanopeptolins, aeruginosins, microviridins) [26]. Several may also be bioactive or even toxic to vertebrates since many are produced through the same metabolic pathway as the MCs [27] and have similar structures [28]. Besides the public and environmental health needs for more research on these co...

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