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| Mccarron, Pearse; Emteborg, Hakan; Nulty, Ciara; Rundberget, Thomas; Loader, Jared I.; Teipel, Katharina; Miles, Christopher O.; Quilliam, Michael A.; Hess, Philipp. |
| The development of multi-analyte methods for lipophilic shellfish toxins based on liquid chromatography-mass spectrometry permits rapid screening and analysis of samples for a wide variety of toxins in a single run. Validated methods and appropriate certified reference materials (CRMs) are required to ensure accuracy of results. CRMs are essential for accurate instrument calibration, for assessing the complete analytical method from sample extraction to data analysis and for verifying trueness. However, CRMs have hitherto only been available for single toxin groups. Production of a CRM containing six major toxin groups was achieved through an international collaboration. Preparation of this material, CRM-FDMT1, drew on information from earlier studies as... |
| Tipo: Text |
Palavras-chave: CRM-FDMT1; Certified reference material; Shellfish toxins; Phycotoxins; Accuracy; Precision; Liquid chromatography-mass spectrometry. |
| Ano: 2011 |
URL: http://archimer.ifremer.fr/doc/00037/14826/12237.pdf |
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| Kilcoyne, Jane; Nulty, Ciara; Jauffrais, Thierry; Mccarron, Pearse; Herve, Fabienne; Foley, Barry; Rise, Frode; Crain, Sheila; Wilkins, Alistair L.; Twiner, Michael J.; Hess, Philipp; Miles, Christopher O.. |
| We identified three new azaspiracids (AZAs) with molecular weights of 715, 815, and 829 (AZA33 (3), AZA34 (4), and AZA35, respectively) in mussels, seawater, and Azadinium spinosum culture. Approximately 700 mu g of 3 and 250 mu g of 4 were isolated from a bulk culture of A. spinosum, and their structures determined by MS and NMR spectroscopy. These compounds differ significantly at the carboxyl end of the molecule from known AZA analogues and therefore provide valuable information on structure-activity relationships. Initial toxicological assessment was performed using an in vitro model system based on Jurkat T lymphocyte cytotoxicity, and the potencies of 3 and 4 were found to be 0.22- and 5.5-fold that of AZA1 (1), respectively. Thus, major changes in... |
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| Ano: 2014 |
URL: https://archimer.ifremer.fr/doc/00245/35606/34414.pdf |
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| Jauffrais, Thierry; Kilcoyne, Jane; Sechet, Veronique; Herrenknecht, Christine; Truquet, Philippe; Herve, Fabienne; Berard, Jean-baptiste; Nulty, Ciara; Taylor, Sarah; Tillmann, Urban; Miles, Christopher O.; Hess, Philipp. |
| Azaspiracid (AZA) poisoning has been reported following consumption of contaminated shellfish, and is of human health concern. Hence, it is important to have sustainable amounts of the causative toxins available for toxicological studies and for instrument calibration in monitoring programs, without having to rely on natural toxin events. Continuous pilot scale culturing was carried out to evaluate the feasibility of AZA production using Azadinium spinosum cultures. Algae were harvested using tangential flow filtration or continuous centrifugation. AZAs were extracted using solid phase extraction (SPE) procedures, and subsequently purified. When coupling two stirred photobioreactors in series, cell concentrations reached 190,000 and 210,000 cell·mL−1 at... |
| Tipo: Text |
Palavras-chave: Solid phase extraction; Photobioreactor; Chemostat; Dinoflagellate; Micro-algae; LC-MS/MS; Tangential flow filtration; Azaspiracid; HP-20. |
| Ano: 2012 |
URL: http://archimer.ifremer.fr/doc/00088/19875/17526.pdf |
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