Abstract
Palytoxin (PlTX) and analogues are produced by certain dinoflagellates, sea anemones, corals and cyanobacteria. PlTX can accumulate in the food chain and when consumed it may cause intoxication with symptoms like myalgia, weakness, fever, nausea, and vomiting. The analysis of PlTXs is challenging, and because of the large molecular structure, it is difficult to develop a sensitive and selective liquid chromatography-mass spectrometry (LC-MS/MS) method. In this work, an LC-MS/MS method was developed to analyse PlTXs with use of lithium iodine and formic acid as additives in the mobile phase. For method development, initially, LC-hrMS was used to accurately determine the elemental composition of the precursor and product ions. The main adduct formed was [M + H + 2Li]3+. Fragments were identified with LC-hrMS and these were incorporated in the LC-MS/MS method. A method of 10 min was developed and a solid phase extraction clean-up procedure was optimised for shellfish matrix. The determined limits of detection were respectively 8 and 22 µg PlTX kg−1 for mussel and oyster matrix. Oysters gave a low recovery of approximately 50% for PlTX during extraction. The method was successfully in-house validated, repeatability had a relative standard deviation less than 20% (n = 5) at 30 µg PlTX kg−1 in mussel, cockle, and ensis, and at 60 µg PlTX kg−1 in oyster.
Highlights
Palytoxin (PlTX), ovatoxin (OVTX), ostreocin, and other analogues are produced by the dinoflagellates Ostreopsis ovata and Ostreopsis siamensis [1,2,3,4] as well as by certain sea anemones, and corals of the Palythoa species and cyanobacteria of the genus Trichodesmium [5,6]
PlTXs can accumulate in the food chain in organisms like mussels, crabs, and fish [8]
Since the discovery of PlTX in the 1960’s, a number of exposures and poisonings related to PlTX have been reported from several parts of the world [11,12]
Summary
Palytoxin (PlTX), ovatoxin (OVTX), ostreocin, and other analogues are produced by the dinoflagellates Ostreopsis ovata and Ostreopsis siamensis [1,2,3,4] as well as by certain sea anemones, and corals of the Palythoa species and cyanobacteria of the genus Trichodesmium [5,6]. The in vivo test has a direct response (mouse death) and proponents believe unknown toxins will be detected by this system The drawback of this test, beside that the method is unethical, is the route of administration, which is i.p. instead of oral. In the hrMS complex spectra were obtained consisting out of multiple adducts with various charge states and in source fragmentation of multiple losses of water The sensitivity of this method is sufficient (limit of quantitation (LOQ) of 44 ng mL−1 in shellfish extract) but can be improved [25,26]. Selwood et al developed a more sensitive method based on a micro oxidation of PlTX to low molecular weight oxidation products [27]. [29,30,31]
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