Miles Christopher O, Burton Ian W, Lewis Nancy I, Robertson Alison, Giddings Sabrina D, McCarron Pearse, Mudge Elizabeth M
Biotoxin Metrology, National Research Council, 1411 Oxford Street, Halifax, NS, B3H 3Z1 Canada.
Norwegian Veterinary Institute, P.O. Box 64, 1431 Ås, Norway.
Tetrahedron. 2024 Aug 3;162. doi: 10.1016/j.tet.2024.134115. Epub 2024 Jun 18.
Ciguatera poisoning occurs throughout subtropical and tropical regions globally. The Virgin Islands in the Caribbean Sea is a known hyperendemic region for ciguatera and has been associated with Caribbean ciguatoxin (C-CTX) contamination in fish. An algal C-CTX (C-CTX5) was identified in and isolated from benthic algal samples collected in waters south St. Thomas, US Virgin Islands. The highest CTX-producing isolate, 1602 SH-6, was grown at large-scale to isolate sufficient C-CTX5 for structural confirmation by NMR spectroscopy. A series of orthogonal extraction and fractionation procedures resulted in purification of approximately 40 μg of C-CTX5, as estimated by quantitative NMR. A suite of 1D and 2D NMR experiments were acquired that verified the structure originally proposed for C-CTX5. The structural confirmation and successful isolation of C-CTX5 opens the way for work on the stability, toxicology and biotransformation of C-CTXs, as well as for the production of quantitative reference materials for analytical method development and validation. The strategies developed for purification of C-CTX5 may also apply to isolation and purification of CTXs from the Pacific Ocean and other regions.
雪卡毒素中毒在全球亚热带和热带地区均有发生。加勒比海的维尔京群岛是已知的雪卡毒素高度流行地区，且与鱼类中的加勒比雪卡毒素（C-CTX）污染有关。从美属维尔京群岛圣托马斯岛以南水域采集的底栖藻类样本中，鉴定出一种藻类C-CTX（C-CTX5）并进行了分离。产量最高的CTX产生菌株1602 SH-6进行了大规模培养，以分离出足够的C-CTX5，用于通过核磁共振光谱进行结构确认。一系列正交提取和分馏程序导致纯化出约40μg的C-CTX5，通过定量核磁共振估算得出。进行了一套一维和二维核磁共振实验，验证了最初为C-CTX5提出的结构。C-CTX5的结构确认和成功分离为研究C-CTXs的稳定性、毒理学和生物转化，以及为分析方法开发和验证生产定量参考物质开辟了道路。为纯化C-CTX5而开发的策略也可能适用于从太平洋和其他地区分离和纯化CTXs。
