Preparative Separation and Purification of Trichothecene Mycotoxins from the Marine Fungus Fusarium sp. LS68 by High-Speed Countercurrent Chromatography in Stepwise Elution Mode

The contamination of foods and animal feeds with trichothecene mycotoxins is a growing concern for human and animal health. As such, large quantities of pure trichothecene mycotoxins are necessary for food safety monitoring and toxicological research. A new and effective method for the purification...

Full description

Bibliographic Details
Main Authors: Yong Liu, Xuezhen Zhou, C. Benjamin Naman, Yanbin Lu, Lijian Ding, Shan He
Format: Article
Language:English
Published: MDPI AG 2018-02-01
Series:Marine Drugs
Subjects:
Online Access:http://www.mdpi.com/1660-3397/16/2/73
_version_ 1811263960356225024
author Yong Liu
Xuezhen Zhou
C. Benjamin Naman
Yanbin Lu
Lijian Ding
Shan He
author_facet Yong Liu
Xuezhen Zhou
C. Benjamin Naman
Yanbin Lu
Lijian Ding
Shan He
author_sort Yong Liu
collection DOAJ
description The contamination of foods and animal feeds with trichothecene mycotoxins is a growing concern for human and animal health. As such, large quantities of pure trichothecene mycotoxins are necessary for food safety monitoring and toxicological research. A new and effective method for the purification of trichothecene mycotoxins from a marine fungus, Fusarium sp. LS68, is described herein. Preparative high-speed countercurrent chromatography (HSCCC) was utilized for the scalable isolation and purification of four trichothecene mycotoxins for the first time in stepwise elution mode, with a biphasic solvent system composed of hexanes–EtOAc–CH3OH–H2O (6:4:5:5, v/v/v/v) and (8.5:1.5:5:5,v/v/v/v). This preparative HSCCC separation was performed on 200 mg of crude sample to yield four trichothecene mycotoxins, roridin E (1), roridin E acetate (2), verrucarin L acetate (3), and verrucarin J (4) in a single run, with each of >98% purity. These compounds were identified by MS, 1H NMR, 13C NMR, and polarimetry. The results demonstrate an efficient HSCCC method for the separation of trichothecene mycotoxins, which can be utilized to produce pure commercial and research standards.
first_indexed 2024-04-12T19:55:48Z
format Article
id doaj.art-96921bc398194adaba76083c8b269903
institution Directory Open Access Journal
issn 1660-3397
language English
last_indexed 2024-04-12T19:55:48Z
publishDate 2018-02-01
publisher MDPI AG
record_format Article
series Marine Drugs
spelling doaj.art-96921bc398194adaba76083c8b2699032022-12-22T03:18:41ZengMDPI AGMarine Drugs1660-33972018-02-011627310.3390/md16020073md16020073Preparative Separation and Purification of Trichothecene Mycotoxins from the Marine Fungus Fusarium sp. LS68 by High-Speed Countercurrent Chromatography in Stepwise Elution ModeYong Liu0Xuezhen Zhou1C. Benjamin Naman2Yanbin Lu3Lijian Ding4Shan He5Li Dak Sum Yip Yio Chin Kenneth Li Marine Biopharmaceutical Research Center, Ningbo University, Ningbo 315211, ChinaLi Dak Sum Yip Yio Chin Kenneth Li Marine Biopharmaceutical Research Center, Ningbo University, Ningbo 315211, ChinaLi Dak Sum Yip Yio Chin Kenneth Li Marine Biopharmaceutical Research Center, Ningbo University, Ningbo 315211, ChinaInstitute of Seafood, Zhejiang Gongshang University, Hangzhou 310012, ChinaLi Dak Sum Yip Yio Chin Kenneth Li Marine Biopharmaceutical Research Center, Ningbo University, Ningbo 315211, ChinaLi Dak Sum Yip Yio Chin Kenneth Li Marine Biopharmaceutical Research Center, Ningbo University, Ningbo 315211, ChinaThe contamination of foods and animal feeds with trichothecene mycotoxins is a growing concern for human and animal health. As such, large quantities of pure trichothecene mycotoxins are necessary for food safety monitoring and toxicological research. A new and effective method for the purification of trichothecene mycotoxins from a marine fungus, Fusarium sp. LS68, is described herein. Preparative high-speed countercurrent chromatography (HSCCC) was utilized for the scalable isolation and purification of four trichothecene mycotoxins for the first time in stepwise elution mode, with a biphasic solvent system composed of hexanes–EtOAc–CH3OH–H2O (6:4:5:5, v/v/v/v) and (8.5:1.5:5:5,v/v/v/v). This preparative HSCCC separation was performed on 200 mg of crude sample to yield four trichothecene mycotoxins, roridin E (1), roridin E acetate (2), verrucarin L acetate (3), and verrucarin J (4) in a single run, with each of >98% purity. These compounds were identified by MS, 1H NMR, 13C NMR, and polarimetry. The results demonstrate an efficient HSCCC method for the separation of trichothecene mycotoxins, which can be utilized to produce pure commercial and research standards.http://www.mdpi.com/1660-3397/16/2/73trichothecene mycotoxinsroridinverrucarinhigh-speed countercurrent chromatographypreparative separationstepwise elution
spellingShingle Yong Liu
Xuezhen Zhou
C. Benjamin Naman
Yanbin Lu
Lijian Ding
Shan He
Preparative Separation and Purification of Trichothecene Mycotoxins from the Marine Fungus Fusarium sp. LS68 by High-Speed Countercurrent Chromatography in Stepwise Elution Mode
Marine Drugs
trichothecene mycotoxins
roridin
verrucarin
high-speed countercurrent chromatography
preparative separation
stepwise elution
title Preparative Separation and Purification of Trichothecene Mycotoxins from the Marine Fungus Fusarium sp. LS68 by High-Speed Countercurrent Chromatography in Stepwise Elution Mode
title_full Preparative Separation and Purification of Trichothecene Mycotoxins from the Marine Fungus Fusarium sp. LS68 by High-Speed Countercurrent Chromatography in Stepwise Elution Mode
title_fullStr Preparative Separation and Purification of Trichothecene Mycotoxins from the Marine Fungus Fusarium sp. LS68 by High-Speed Countercurrent Chromatography in Stepwise Elution Mode
title_full_unstemmed Preparative Separation and Purification of Trichothecene Mycotoxins from the Marine Fungus Fusarium sp. LS68 by High-Speed Countercurrent Chromatography in Stepwise Elution Mode
title_short Preparative Separation and Purification of Trichothecene Mycotoxins from the Marine Fungus Fusarium sp. LS68 by High-Speed Countercurrent Chromatography in Stepwise Elution Mode
title_sort preparative separation and purification of trichothecene mycotoxins from the marine fungus fusarium sp ls68 by high speed countercurrent chromatography in stepwise elution mode
topic trichothecene mycotoxins
roridin
verrucarin
high-speed countercurrent chromatography
preparative separation
stepwise elution
url http://www.mdpi.com/1660-3397/16/2/73
work_keys_str_mv AT yongliu preparativeseparationandpurificationoftrichothecenemycotoxinsfromthemarinefungusfusariumspls68byhighspeedcountercurrentchromatographyinstepwiseelutionmode
AT xuezhenzhou preparativeseparationandpurificationoftrichothecenemycotoxinsfromthemarinefungusfusariumspls68byhighspeedcountercurrentchromatographyinstepwiseelutionmode
AT cbenjaminnaman preparativeseparationandpurificationoftrichothecenemycotoxinsfromthemarinefungusfusariumspls68byhighspeedcountercurrentchromatographyinstepwiseelutionmode
AT yanbinlu preparativeseparationandpurificationoftrichothecenemycotoxinsfromthemarinefungusfusariumspls68byhighspeedcountercurrentchromatographyinstepwiseelutionmode
AT lijianding preparativeseparationandpurificationoftrichothecenemycotoxinsfromthemarinefungusfusariumspls68byhighspeedcountercurrentchromatographyinstepwiseelutionmode
AT shanhe preparativeseparationandpurificationoftrichothecenemycotoxinsfromthemarinefungusfusariumspls68byhighspeedcountercurrentchromatographyinstepwiseelutionmode