Profiling of Brevetoxin Metabolites Produced by <i>Karenia brevis</i> 165 Based on Liquid Chromatography-Mass Spectrometry

In this study, <i>Karenia brevis</i> 165 (<i>K. brevis</i> 165), a Chinese strain, was used to research brevetoxin (BTX) metabolites. The sample pretreatment method for the enrichment of BTX metabolites in an algal culture medium was improved here. The method for screening an...

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Main Authors: Huihui Shen, Xiuxian Song, Yue Zhang, Peipei Zhang, Jing Li, Weijia Song, Zhiming Yu
Format: Article
Language:English
Published: MDPI AG 2021-05-01
Series:Toxins
Subjects:
Online Access:https://www.mdpi.com/2072-6651/13/5/354
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author Huihui Shen
Xiuxian Song
Yue Zhang
Peipei Zhang
Jing Li
Weijia Song
Zhiming Yu
author_facet Huihui Shen
Xiuxian Song
Yue Zhang
Peipei Zhang
Jing Li
Weijia Song
Zhiming Yu
author_sort Huihui Shen
collection DOAJ
description In this study, <i>Karenia brevis</i> 165 (<i>K. brevis</i> 165), a Chinese strain, was used to research brevetoxin (BTX) metabolites. The sample pretreatment method for the enrichment of BTX metabolites in an algal culture medium was improved here. The method for screening and identifying intracellular and extracellular BTX metabolites was established based on liquid chromatography-time-of-flight mass spectrometry (LC-ToF-MS) and liquid chromatography triple quadrupole tandem mass spectrometry (LC-QqQ-MS/MS). The results show that the recovery rates for BTX toxins enriched by a hydrophilic–lipophilic balance (HLB) extraction column were higher than those with a C18 extraction column. This method was used to analyze the profiles of extracellular and intracellular BTX metabolites at different growth stages of <i>K. brevis</i> 165. This is the first time a Chinese strain of <i>K. brevis</i> has been reported that can produce toxic BTX metabolites. Five and eight kinds of BTX toxin metabolites were detected in the cell and culture media of <i>K. brevis</i> 165, respectively. Brevenal, a toxic BTX metabolite antagonist, was found for the first time in the culture media. The toxic BTX metabolites and brevenal in the <i>K. brevis</i> 165 cell and culture media were found to be fully proven in terms of the necessity of establishing a method for screening and identifying toxic BTX metabolites. The results found by qualitatively and quantitatively analyzing BTX metabolites produced by <i>K. brevis</i> 165 at different growth stages show that the total toxic BTX metabolite contents in single cells ranged between 6.78 and 21.53 pg/cell, and the total toxin concentration in culture media ranged between 10.27 and 449.11 μg/L. There were significant differences in the types and contents of toxic BTX metabolites with varying growth stages. Therefore, when harmful algal blooms occur, the accurate determination of BTX metabolite types and concentrations will be helpful to assess the ecological disaster risk in order to avoid hazards and provide appropriate disaster warnings.
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spelling doaj.art-6fae3c672fe9463cbb8d797241e12a462023-11-21T19:50:30ZengMDPI AGToxins2072-66512021-05-0113535410.3390/toxins13050354Profiling of Brevetoxin Metabolites Produced by <i>Karenia brevis</i> 165 Based on Liquid Chromatography-Mass SpectrometryHuihui Shen0Xiuxian Song1Yue Zhang2Peipei Zhang3Jing Li4Weijia Song5Zhiming Yu6CAS Key Laboratory of Marine Ecology and Environmental Sciences, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, ChinaCAS Key Laboratory of Marine Ecology and Environmental Sciences, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, ChinaCAS Key Laboratory of Marine Ecology and Environmental Sciences, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, ChinaCAS Key Laboratory of Marine Ecology and Environmental Sciences, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, ChinaCAS Key Laboratory of Marine Ecology and Environmental Sciences, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, ChinaCAS Key Laboratory of Marine Ecology and Environmental Sciences, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, ChinaCAS Key Laboratory of Marine Ecology and Environmental Sciences, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, ChinaIn this study, <i>Karenia brevis</i> 165 (<i>K. brevis</i> 165), a Chinese strain, was used to research brevetoxin (BTX) metabolites. The sample pretreatment method for the enrichment of BTX metabolites in an algal culture medium was improved here. The method for screening and identifying intracellular and extracellular BTX metabolites was established based on liquid chromatography-time-of-flight mass spectrometry (LC-ToF-MS) and liquid chromatography triple quadrupole tandem mass spectrometry (LC-QqQ-MS/MS). The results show that the recovery rates for BTX toxins enriched by a hydrophilic–lipophilic balance (HLB) extraction column were higher than those with a C18 extraction column. This method was used to analyze the profiles of extracellular and intracellular BTX metabolites at different growth stages of <i>K. brevis</i> 165. This is the first time a Chinese strain of <i>K. brevis</i> has been reported that can produce toxic BTX metabolites. Five and eight kinds of BTX toxin metabolites were detected in the cell and culture media of <i>K. brevis</i> 165, respectively. Brevenal, a toxic BTX metabolite antagonist, was found for the first time in the culture media. The toxic BTX metabolites and brevenal in the <i>K. brevis</i> 165 cell and culture media were found to be fully proven in terms of the necessity of establishing a method for screening and identifying toxic BTX metabolites. The results found by qualitatively and quantitatively analyzing BTX metabolites produced by <i>K. brevis</i> 165 at different growth stages show that the total toxic BTX metabolite contents in single cells ranged between 6.78 and 21.53 pg/cell, and the total toxin concentration in culture media ranged between 10.27 and 449.11 μg/L. There were significant differences in the types and contents of toxic BTX metabolites with varying growth stages. Therefore, when harmful algal blooms occur, the accurate determination of BTX metabolite types and concentrations will be helpful to assess the ecological disaster risk in order to avoid hazards and provide appropriate disaster warnings.https://www.mdpi.com/2072-6651/13/5/354<i>Karenia brevis</i> 165profilebrevetoxin metabolitesliquid chromatography-mass spectrometry
spellingShingle Huihui Shen
Xiuxian Song
Yue Zhang
Peipei Zhang
Jing Li
Weijia Song
Zhiming Yu
Profiling of Brevetoxin Metabolites Produced by <i>Karenia brevis</i> 165 Based on Liquid Chromatography-Mass Spectrometry
Toxins
<i>Karenia brevis</i> 165
profile
brevetoxin metabolites
liquid chromatography-mass spectrometry
title Profiling of Brevetoxin Metabolites Produced by <i>Karenia brevis</i> 165 Based on Liquid Chromatography-Mass Spectrometry
title_full Profiling of Brevetoxin Metabolites Produced by <i>Karenia brevis</i> 165 Based on Liquid Chromatography-Mass Spectrometry
title_fullStr Profiling of Brevetoxin Metabolites Produced by <i>Karenia brevis</i> 165 Based on Liquid Chromatography-Mass Spectrometry
title_full_unstemmed Profiling of Brevetoxin Metabolites Produced by <i>Karenia brevis</i> 165 Based on Liquid Chromatography-Mass Spectrometry
title_short Profiling of Brevetoxin Metabolites Produced by <i>Karenia brevis</i> 165 Based on Liquid Chromatography-Mass Spectrometry
title_sort profiling of brevetoxin metabolites produced by i karenia brevis i 165 based on liquid chromatography mass spectrometry
topic <i>Karenia brevis</i> 165
profile
brevetoxin metabolites
liquid chromatography-mass spectrometry
url https://www.mdpi.com/2072-6651/13/5/354
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