Determination of okadaic acid, dinophysistoxin-1 and related esters in Greek mussels using HPLC with fluorometric detection, LC-MS/MS and mouse bioassay
Determination of okadaic acid, dinophysistoxin-1 and related esters in Greek mussels using HPLC with fluorometric detection, LC-MS/MS and mouse bioassay
(EN)
Louppis, A. P.
(EN)
Πανεπιστήμιο Ιωαννίνων. Σχολή Θετικών Επιστημών. Τμήμα Χημείας
(EL)
Louppis, A. P.
(EN)
An approach involving both chemical and biological methods was undertaken for the detection and quantification of the marine toxins okadaic acid (OA), dinophysistoxin-1 (DTX-1) and their respective esters in mussels from different sampling sites in Greece during the period 2006-2007. Samples were analyzed by means of a) high performance liquid chromatography with fluorometric detection (HPLC-FLD), using 9-athryldiazomethane (ADAM), as a pre-column derivatization reagent, b) liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) and c) the mouse bioassay. Free OA and DTX-1 were determined by both HPLC-FLD and LC-MS/MS, while their respective esters were determined only by LC-MS/MS after alkaline hydrolysis of the samples. The detection limit (L.O.D.) and quantification limit (L.O.Q) of the HPLC-FLD method were 0.015 mu g/g HP and 0.050 mu g/g HP, respectively, for OA. The detection limit (L.O.D.) and quantification limit (L.O.Q.) of the LC-MS/MS method were 0.045 mu g/g HP and 0.135 mu g/g HP, respectively, for OA. Comparison of results between the two analytical methods showed excellent agreement (100%), while both HPLC-FLD and LC-MS/MS methods showed an agreement of 97.1% compared to the mouse bioassay. (C) 2009 Elsevier Ltd. All rights reserved.
(EN)
