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A Sensitive LC-MS/MS Method for Palytoxin Using Lithium Cationization

RIKILT, Wageningen University and Research Center, Akkermaalsbos 2, 6708 WB Wageningen, The Netherlands
Authors to whom correspondence should be addressed.
Toxins 2018, 10(12), 537;
Received: 30 October 2018 / Revised: 10 December 2018 / Accepted: 11 December 2018 / Published: 14 December 2018
(This article belongs to the Special Issue Emerging Marine Biotoxins)
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. View Full-Text
Keywords: palytoxin; ovatoxins; mass spectrometry; cationization palytoxin; ovatoxins; mass spectrometry; cationization
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MDPI and ACS Style

Klijnstra, M.D.; Gerssen, A. A Sensitive LC-MS/MS Method for Palytoxin Using Lithium Cationization. Toxins 2018, 10, 537.

AMA Style

Klijnstra MD, Gerssen A. A Sensitive LC-MS/MS Method for Palytoxin Using Lithium Cationization. Toxins. 2018; 10(12):537.

Chicago/Turabian Style

Klijnstra, Mirjam D., and Arjen Gerssen. 2018. "A Sensitive LC-MS/MS Method for Palytoxin Using Lithium Cationization" Toxins 10, no. 12: 537.

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