Toward Isolation of Palytoxins: Liquid Chromatography Coupled to Low- or High-Resolution Mass Spectrometry for the Study on the Impact of Drying Techniques, Solvents and Materials

Type Article
Date 2021-09
Language English
Author(s) Mazzeo Antonia1, Varra Michela1, Tartaglione Luciana1, 2, Ciminiello Patrizia1, Zendong Zita3, Hess PhilippORCID3, Dell'Aversano Carmela1, 2
Affiliation(s) 1 : Department of Pharmacy, School of Medicine and Surgery, University of Napoli Federico II, Via D. Montesano 49, 80131 Napoli, Italy
2 : CoNISMa—National Inter-University Consortium for Marine Sciences, Piazzale Flaminio 9, 00196 Rome, Italy
3 : Ifremer, DYNECO, Laboratoire Phycotoxines, Rue de l’Île d’Yeu, 44311 Nantes, France
Source Toxins (2072-6651) (MDPI), 2021-09 , Vol. 13 , N. 9 , P. 650 (18p.)
DOI 10.3390/toxins13090650
WOS© Times Cited 2
Note This article belongs to the Section Marine and Freshwater Toxins
Keyword(s) palytoxin, LC-HRMS, evaporation, stability, palytoxin methyl ester
Abstract

Palytoxin (PLTX) and its congeners are emerging toxins held responsible for a number of human poisonings following the inhalation of toxic aerosols, skin contact, or the ingestion of contaminated seafood. Despite the strong structural analogies, the relative toxic potencies of PLTX congeners are quite different, making it necessary to isolate them individually in sufficient amounts for toxicological and analytical purposes. Previous studies showed poor PLTX recoveries with a dramatic decrease in PLTX yield throughout each purification step. In view of a large-scale preparative work aimed at the preparation of PLTX reference material, we have investigated evaporation as a critical—although unavoidable—step that heavily affects overall recoveries. The experiments were carried out in two laboratories using different liquid chromatography-mass spectrometry (LC-MS) instruments, with either unit or high resolution. Palytoxin behaved differently when concentrated to a minimum volume rather than when evaporated to complete dryness. The recoveries strongly depended on the solubility as well as on the material of the used container. The LC-MS analyses of PLTX dissolved in aqueous organic blends proved to give a peak intensity higher then when dissolved in pure water. After drying, the PLTX adsorption appeared stronger on glass surfaces than on plastic materials. However, both the solvents used to dilute PLTX and that used for re-dissolution had an important role. A quantitative recovery (97%) was achieved when completely drying 80% aqueous EtOH solutions of PLTX under N2-stream in Teflon. The stability of PLTX in acids was also investigated. Although PLTX was quite stable in 0.2% acetic acid solutions, upon exposure to stronger acids (pH < 2.66), degradation products were observed, among which a PLTX methyl-ester was identified

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How to cite 

Mazzeo Antonia, Varra Michela, Tartaglione Luciana, Ciminiello Patrizia, Zendong Zita, Hess Philipp, Dell'Aversano Carmela (2021). Toward Isolation of Palytoxins: Liquid Chromatography Coupled to Low- or High-Resolution Mass Spectrometry for the Study on the Impact of Drying Techniques, Solvents and Materials. Toxins, 13(9), 650 (18p.). Publisher's official version : https://doi.org/10.3390/toxins13090650 , Open Access version : https://archimer.ifremer.fr/doc/00722/83390/