Stability and Chemical Conversion of the Purified Reference Material of Gymnodimine-A under Different Temperature and pH Conditions

Type Article
Date 2022-11
Language English
Author(s) Wang Guixiang1, Qiu Jiangbing1, 2, Li AifengORCID1, 2, Ji Ying1, Tang Zhixuan1, Hess PhilippORCID3
Affiliation(s) 1 : College of Environmental Science and Engineering, Ocean University of China, Qingdao 266100, China
2 : Key Laboratory of Marine Environment and Ecology, Ocean University of China, Ministry of Education, Qingdao 266100, China
3 : Ifremer, PHYTOX Research Unit, F-44000 Nantes, France
Source Toxins (2072-6651) (MDPI AG), 2022-11 , Vol. 14 , N. 11 , P. 744 (14p.)
DOI 10.3390/toxins14110744
Note This article belongs to the Section Marine and Freshwater Toxins
Keyword(s) gymnodimines (GYMs), stability, chemical conversion, liquid chromatography-high resolution mass spectrometry (LC-HRMS), certified reference materials (CRMs)

Gymnodimines (GYMs) are a group of fast-acting phycotoxins and their toxicological effects on human beings are still unclear due to the lack of sufficiently well-characterized large quantities of purified toxins for toxicology studies. In this study, a certified reference material (CRM) of GYM-A was prepared from the dinoflagellate Karenia selliformis, followed by multi-step chromatography separation and purification. Subsequently, the stability of GYM-A in methanolic media was evaluated at different temperature (−20, 4, and 20 °C) and pH (3, 5, and 7) conditions for 8 months, and the conversion products of GYM-A were explored by liquid chromatography–high resolution mass spectrometry (LC-HRMS). The results show that the stability of GYM-A decreased with increasing temperature and pH values. The GYM-A was stable during storage at −20 °C regardless of pH, but it decreased rapidly (81.8% ± 9.3%) at 20 °C in pH 7 solution after 8 months. Moreover, the concentrations of GYM-A did not significantly change at all temperatures in solutions with pH 3 (p > 0.05). It is recommended that GYM-A should be stored at low temperature (≤−20 °C) and pH (≤3) conditions for long-term storage in aqueous methanolic media. In addition, two conversion products of GYM-A, tentatively named as GYM-K (m/z 540) and GYM-L (m/z 524), were identified in the samples stored at high levels of pH and temperature. Based on the LC-HRMS data, the hypothetical chemical structures of both converting derivatives were proposed. A useful strategy for long-term storage of GYM-A CRM in aqueous methanolic media was suggested and two hypothesized conversion products of GYM-A were discovered in this study.

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