Characterisation of okadaic acid related toxins by liquid chromatography coupled with mass spectrometry

Paz, Beatriz; Daranas, Antonio Hernández; Cruz, Patricia G.; Franco, José M.; Pizarro, Gemita; Souto, Marı́a L.; Norte, Manuel; Fernández, José J.

doi:10.1016/j.toxicon.2007.03.015

Cited by 33 publications

(23 citation statements)

References 26 publications

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“…Absence of sulphated forms was confirmed in cultures of P. lima (strain PL2V) (Paz et al 2007). In contrast, large amounts of DTX5c-like sulphated toxins were found in cultures of P. belizeanum (strain PBMA01) grown under the same experimental conditions and with the application of identical toxin-extraction procedures (Cruz et al 2006).…”

Section: Considerations On Diol-ester Production Bymentioning

confidence: 87%

“…Negative mode was performed to confirm the toxin spectra. To search for the presence of sulphated forms of dinophysistoxin-4 (DTX4) and dinophysistoxin-5b (DTX5b), derived from OA-D8, m/z for our adduct ions were calculated from Hu et al (1995a) and Paz et al (2007). We also sought the presence of OA diol-esters with C7 and C9 side chain, whose m/z were calculated for our adduct ions from Suzuki et al (2004).…”

Section: Methodsmentioning

confidence: 99%

“…Quantified DTX2 (6 μg ml ) and PTX1 (10 μg ml -1 ) reference materials were provided by colleagues (see 'Acknowledgements'). Qualitative reference material of OA-D8 diol-ester (OA-D8) was prepared from cultures of Prorocentrum lima (Paz et al 2007).…”

Section: Methodsmentioning

confidence: 99%

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Growth, behaviour and cell toxin quota of Dinophysis acuta during a daily cycle

Pizarro

Escalera²,

González-Gil³

et al. 2008

Mar. Ecol. Prog. Ser.

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), a high frequency of dead cells (up to 15%) and cells with starch granules (up to 93%), and no evidence of recent mixotrophic behaviour. Still, the cells, which did not perform vertical migration, aggregated around salinity-driven density discontinuities in the top 5 m and had a high cell toxin quota (determined by liquid chromatography-mass spectrometry) for this species. A 3.5-fold difference was found between maximum (during the night) and minimum values of cell toxin quota. Okadaic acid (OA) was the predominant toxin and changes in cell quota of different toxins showed different daily patterns in the content of okadaiates and pectenotoxins; thus, the toxin profile is influenced by the time of sampling. Dissolved toxins (adsorbed by resins in passive samplers from 8 to 14 November) also reached annual maxima and reflected the vertical distribution of D. acuta cells. These results emphasize the need to parameterize physiological conditions and behaviour of Dinophysis populations during different phases of the population growth and hydrodynamic scenarios.

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Section: Considerations On Diol-ester Production Bymentioning

confidence: 87%

Section: Methodsmentioning

confidence: 99%

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Growth, behaviour and cell toxin quota of Dinophysis acuta during a daily cycle

Pizarro

Escalera²,

González-Gil³

et al. 2008

Mar. Ecol. Prog. Ser.

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“…Operating the software programme ToxID 2.1.2 (Thermo Fisher Scientific, San José, USA), the full-scan data of three culture extracts were efficiently screened. To this end, a ToxID database from Gerssen et al [15] was modified by adding new compounds and molecular formulas of 98 relevant toxins [24,[50][51][52][53][54][55][56][57][58][59][60][61][62], see Table S1 …”

Section: Algal Toxin Profilementioning

confidence: 99%

Quantification and profiling of lipophilic marine toxins in microalgae by UHPLC coupled to high-resolution orbitrap mass spectrometry

et al. 2015

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During the last decade, a significant increase in the occurrence of harmful algal blooms (HABs), linked to repetitive cases of shellfish contamination has become a public health concern and therefore, accurate methods to detect marine toxins in different matrices are required. In this study, we developed a method for profiling lipophilic marine microalgal toxins based on ultra-high-performance liquid chromatography coupled to high-resolution Orbitrap mass spectrometry (UHPLC-HR-Orbitrap MS). Extraction of selected toxins (okadaic acid (OA), dinophysistoxin-1 (DTX-1), pectenotoxin-2 (PTX-2), azaspiracid-1 (AZA-1), yessotoxin (YTX) and 13-desmethyl spirolide C (SPX-1)) was optimized using a Plackett-Burman design. Three key algal species, i.e., Prorocentrum lima, Protoceratium reticulatum and Alexandrium ostenfeldii were used to test the extraction efficiency of OA, YTXs and SPXs, respectively. Prorocentrum micans, fortified with certified reference solutions, was used for recovery studies. The quantitative and confirmatory performance of the method was evaluated according to CD 2002/657/EC. Limits of detection and quantification ranged between 0.006 and 0.050 ng mL(-1) and 0.018 to 0.227 ng mL(-1), respectively. The intra-laboratory reproducibility ranged from 6.8 to 11.7 %, repeatability from 6.41 to 11.5 % and mean corrected recoveries from 81.9 to 119.6 %. In addition, algae cultures were retrospectively screened for analogues and metabolites through a homemade database. Using the ToxID software programme, 18 toxin derivates were detected in the extract of three toxin producing microalgae species. In conclusion, the generic extraction and full-scan HRMS approach offers an excellent quantitative performance and simultaneously allows to profile analogues and metabolites of marine toxins in microalgae. Graphical Abstract Optimization of extraction, detection and quantification of lipophilic marine toxins in microalgae by UHPLC-HR Orbitrap MS.

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“…In spite of the high cost of the equipment, LC-MS technique has been successful in control laboratories because of the wealth of information it provides, as well as for its versatility, since it can be used to detect many different types of marine toxins [8]. Therefore, considerable advances to increase the number of targets for the analysis of contaminated shellfish have been made, especially since the use of extracts obtained from cultures of dinoflagellates were introduced [9][10][11]. Okadaic acid (1) 19-epi-Okadaic acid (2).…”

Section: Introductionmentioning

confidence: 99%

Identification of 19-epi-okadaic Acid, a New Diarrhetic Shellfish Poisoning Toxin, by Liquid Chromatography with Mass Spectrometry Detection

et al. 2008

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Okadaic acid (1) (OA) and its congeners are mainly responsible for diarrhetic shellfish poisoning (DSP) syndrome. The presence of several OA derivatives have already been confirmed in Prorocentrum and Dinophysis spp. In this paper, we report on the detection and identification of a new DSP toxin, the OA isomer 19-epi-okadaic acid (2) (19-epi-OA), isolated from cultures of Prorocentrum belizeanum, by determining its retention time (RT) and fragmentation pattern using liquid chromatography coupled with mass spectrometry (LC-MS/MS).

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Characterisation of okadaic acid related toxins by liquid chromatography coupled with mass spectrometry

Cited by 33 publications

References 26 publications

Growth, behaviour and cell toxin quota of Dinophysis acuta during a daily cycle

Growth, behaviour and cell toxin quota of Dinophysis acuta during a daily cycle

Quantification and profiling of lipophilic marine toxins in microalgae by UHPLC coupled to high-resolution orbitrap mass spectrometry

Identification of 19-epi-okadaic Acid, a New Diarrhetic Shellfish Poisoning Toxin, by Liquid Chromatography with Mass Spectrometry Detection

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