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| Poyer, Salome; Loutelier-bourhis, Corinne; Coadou, Gael; Mondeguer, Florence; Enche, Julien; Bossee, Anne; Hess, Philipp; Afonso, Carlos. |
| The aim of this work was to develop a reliable and efficient analytical method to characterise and differentiate saxitoxin analogues (STX), including sulphated (gonyautoxins, GTX) and non-sulphated analogues. For this purpose, hydrophilic interaction liquid chromatography (HILIC) was used to separate sulphated analogues. We also resorted to ion mobility spectrometry to differentiate the STX analogues because this technique adds a new dimension of separation based on ion gas phase conformation. Positive and negative ionisation modes were used for gonyautoxins while positive ionisation mode was used for non-sulphated analogues. Subsequently, the coupling of these three complementary techniques, HILIC-IM-MS, permitted the separation and identification of STX... |
| Tipo: Text |
Palavras-chave: Saxitoxin; Ion mobility-mass spectrometry; Isomers; Multidimensional separation; HILIC. |
| Ano: 2015 |
URL: https://archimer.ifremer.fr/doc/00249/36067/34924.pdf |
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| Poyer, Salome; Loutelier-bourhis, Corinne; Tognetti, Vincent; Joubert, Laurent; Enche, Julien; Bossee, Anne; Mondeguer, Florence; Hess, Philipp; Afonso, Carlos. |
| Gonyautoxins are potent natural neurotoxic analogues of saxitoxin. Due to their biological activity and submilligram lethal dose for man, fast and efficient methods are required for their characterization. Recent advances in ion mobility-mass spectrometry (IM-MS) showed that differentiation of isomers could be achieved using specific experimental conditions involving particular buffer gases as well as cationic species. In this work, IM-MS experiments were carried out using alkali metal ions (Met = Li+, Na+ or K+) and different buffer gases (N2, N2O and CO2) to improve the differentiation of gonyautoxin isomers. The separation of [GTX + Met]+ ion was achieved for GTX2/3 and GTX1/4 from their Na or K adducts. For dcGTX2/3, the ion mobility separation can... |
| Tipo: Text |
Palavras-chave: Ion mobility; Gonyautoxin; Collision cross-section; Alkali adduct. |
| Ano: 2016 |
URL: http://archimer.ifremer.fr/doc/00317/42863/42291.pdf |
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| Poyer, Salomé; Loutelier-bourhis, Corinne; Mondeguer, Florence; Coadou, Gaël; Hubert-roux, Marie; Enche, Julien; Bossee, Anne; Hess, Philipp; Afonso, Carlos. |
| Saxitoxin and its analogues also called paralytic shellfish poisons (PSPs) are very potent neurotoxins [1] produced by dinoflagellates and referenced as chemical weapon in the chemical warfare convention (CWC). The official detection methods for these toxins present limitations concerning their speed and reliability [2]. Due to the presence of isomers, not differentiable by mass spectrometry (MS), an upstream separation is necessary. In order to separate saxitoxin analogues, hydrophilic interaction liquid chromatography (HILIC) and ion mobility (IM) were used. Those techniques respectively developed for high polar compounds and three dimensional structure differentiation are particularly well adapted to the separation of PSPs. This HILIC/IM-MS coupling... |
| Tipo: Text |
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| Ano: 2013 |
URL: http://archimer.ifremer.fr/doc/00179/29039/27475.pdf |
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