FN Archimer Export Format
PT J
TI Characterization of ovatoxin-h, a new ovatoxin analog, and evaluation of chromatographic columns for ovatoxin analysis and purification
BT 
AF BRISSARD, Charline
   HERVE, Fabienne
   SIBAT, Manoella
   SECHET, Veronique
   HESS, Philipp
   AMZIL, Zouher
   HERRENKNECHT, Christine
AS 1:1;2:1;3:1;4:1;5:1;6:1;7:2;
FF 1:PDG-ODE-LITTORAL-PHYC;2:PDG-ODE-LITTORAL-PHYC;3:PDG-ODE-LITTORAL-PHYC;4:PDG-ODE-LITTORAL-PHYC;5:PDG-ODE-LITTORAL-PHYC;6:PDG-ODE-LITTORAL-PHYC;7:;
C1 Ifremer, Phycotoxins Laboratory, rue de l’Ile d’Yeu, BP 21105, F-44311 Nantes, France
   LUNAM, University of Nantes, MMS EA2160, Pharmacy Faculty, 9 rue Bias, F-44035 Nantes, France
C2 IFREMER, FRANCE
   UNIV NANTES, FRANCE
SI NANTES
SE PDG-ODE-LITTORAL-PHYC
IN WOS Ifremer jusqu'en 2018
   copubli-france
   copubli-univ-france
IF 3.926
TC 54
UR https://archimer.ifremer.fr/doc/00252/36302/34831.pdf
LA English
DT Article
DE ;Ostreopsis cf. ovata;palytoxin;ovatoxins;U-HPLC/HR-MSn;chromatographic separation
AB The presence of Ostreopsis cf. ovata on the Mediterranean coast represents a serious concern to human health due to production of toxins–putative palytoxin and ovatoxins (ovatoxin-a, -b, -c, -d, -e, -f and -g). However, purified ovatoxins are not widely available and their toxicities are still unknown. In the present study, we report on HR LC-MS/MS analysis of a French Ostreopsis cf. ovata strain (IFR-OST-0.3 V) collected at Villefranche-sur-Mer (France) during a bloom in 2011. Investigation of this strain of Ostreopsis cf. ovata cultivated in our laboratory by ultra-high performance liquid chromatography coupled to high resolution mass spectrometry (UHPLC-HRMS) confirmed the production of ovatoxins -a to–e and revealed the presence of a new ovatoxin analogue, named ovatoxin-h. Ostreopsis cf. ovata extracts were pre-purified by Sephadex LH-20 to obtain a concentrated fraction of ovatoxins (OVTXs). This method provided a recovery of about 85% of OVTXs and a cleanup efficiency of 93%. Different stationary phases were tested with this fraction of interest to elucidate the structure of the new OVTX congener and to obtain purified ovatoxins. Eight reversed phase sorbents were evaluated for their capacity to separate and purify ovatoxins. Among them Kinetex C18, Kinetex PFP and Uptisphere C18-TF allowed for best separations almost achieving baseline resolution. Kinetex C18 is able to sufficiently separate these toxins, allowing us to identify the toxins present in the extract purified by Sephadex LH-20, and to partly elucidate the structure of the new ovatoxin congener. This toxin possesses one oxygen atom less and two hydrogens more than ovatoxin-a. Investigations using liquid chromatography coupled to high resolution tandem mass spectrometry suggest that the part of the molecule where ovatoxin-h differs from ovatoxin-a is situated between C42 and C49. Uptisphere C18-TF was proposed as a first step preparative chromatography as it is able to separate a higher number of ovatoxins (especially ovatoxin-d and ovatoxin-e) and because it separates ovatoxins from unknown compounds, identified using full scan single quadrupole mass spectrometry. After pre-purification with Sephadex LH-20, purification and separation of individual ovatoxins was attempted using an Uptisphere C18-TF column. During recovery of purified toxins, problems of stability of OVTXs were observed, leading us to investigate experimental conditions responsible for this degradation.
PY 2015
PD APR
SO Journal of Chromatography A
SN 0021-9673
PU Elsevier
VL 1388
UT 000351792400011
BP 87
EP 101
DI 10.1016/j.chroma.2015.02.015
ID 36302
ER

EF