Identification and separation of saxitoxins using hydrophilic interaction liquid chromatography coupled to traveling wave ion mobility-mass spectrometry

Type Article
Date 2015-01
Language English
Author(s) Poyer Salome1, 2, Loutelier-Bourhis Corinne1, 2, Coadou Gael1, 2, Mondeguer FlorenceORCID3, Enche Julien4, Bossee Anne4, Hess PhilippORCID3, Afonso Carlos1, 2
Affiliation(s) 1 : Normandie Univ, COBRA, UMR 6014, F-76821 Mont St Aignan, France.
2 : Univ Rouen, INSA Rouen, CNRS, IRCOF,FR 3038, F-76821 Mont St Aignan, France.
3 : IFREMER, Lab Phycotoxines, F-44311 Nantes 03, France.
4 : DGA Maitrise NRBC, Dept Anal Chim, F-91710 Vert Le Petit, France.
Source Journal Of Mass Spectrometry (1076-5174) (Wiley-blackwell), 2015-01 , Vol. 50 , N. 1 , P. 175-181
DOI 10.1002/jms.3515
WOS© Times Cited 17
Keyword(s) saxitoxin, ion mobility-mass spectrometry, isomers, multidimensional separation, HILIC
Abstract 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 analogues; isomer differentiation was achieved in HILIC dimension while non-sulphated analogues were separated in the IM-MS dimension. Additional structural characteristics concerning the conformation of STXs could be obtained using IM-MS measurements. Thus, the collision cross sections (CCS) of STXs are reported for the first time in the positive ionisation mode. These experimental CCSs correlated well with the calculated CCS values using the trajectory method.
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Poyer Salome, Loutelier-Bourhis Corinne, Coadou Gael, Mondeguer Florence, Enche Julien, Bossee Anne, Hess Philipp, Afonso Carlos (2015). Identification and separation of saxitoxins using hydrophilic interaction liquid chromatography coupled to traveling wave ion mobility-mass spectrometry. Journal Of Mass Spectrometry, 50(1), 175-181. Publisher's official version : https://doi.org/10.1002/jms.3515 , Open Access version : https://archimer.ifremer.fr/doc/00249/36067/