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.
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.
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分离沙冬青毒素：液相色谱-低分辨率或高分辨率质谱联用技术，用于研究干燥技术、溶剂和材料的影响。
DOI：
10.3390/toxins13090650
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发表时间：
2021-09-14
期刊：
影响因子：
4.2
通讯作者：
Dell'Aversano C
中科院分区：
文献类型：
--
作者：
Mazzeo A;Varra M;Tartaglione L;Ciminiello P;Zendong Z;Hess P;Dell'Aversano C
Palytoxin （PLTX）及其同系物是一种新出现的毒素，在吸入有毒气溶胶、皮肤接触或摄入受污染的海鲜后，导致了许多人类中毒。尽管具有很强的结构相似性，但PLTX同源物的相对毒性却大不相同，因此有必要单独分离出足够数量的PLTX同源物，以用于毒理学和分析目的。先前的研究表明，在每个纯化步骤中，PLTX回收率很低，PLTX产量急剧下降。鉴于大规模的准备工作旨在制备PLTX标准物质，我们研究了蒸发作为一个关键的-虽然不可避免的-严重影响整体回收率的步骤。实验在两个实验室进行，使用不同的液相色谱-质谱（LC-MS）仪器，有单位分辨率和高分辨率。当浓缩到最小体积时，与蒸发到完全干燥时，孢毒素的表现不同。回收率很大程度上取决于溶解度和所用容器的材料。液相色谱-质谱分析表明，溶解在有机水溶液中的PLTX峰强度高于溶解在纯水中的PLTX峰强度。干燥后，PLTX在玻璃表面的吸附比在塑料材料表面的吸附更强。然而，用于稀释PLTX的溶剂和用于再溶解的溶剂都起着重要作用。当在n2流中完全干燥80%的PLTX EtOH水溶液时，在Teflon中实现了定量回收率（97%）。还考察了PLTX在酸中的稳定性。虽然PLTX在0.2%醋酸溶液中相当稳定，但在较强酸（pH < 2.66）中，观察到降解产物，其中鉴定出PLTX甲酯。
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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影响因子：
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作者：
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