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Simultaneous determination of biotoxins DSP and AZAs in bivalve molluscs and fish by liquid chromatography/tandem mass spectrometry

Authors

  • Liyang Zhuo,

    1. Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety (Fuzhou University), Fujian Province Key Laboratory of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou, China
    2. Quality Inspection Institute of Quanzhou, Quanzhou, Fujian, China
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  • Wusheng Fu,

    1. Fujian Center for disease Control and Prevention, Fuzhou, Fujian, China
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  • Yiqiang Yang,

    1. Quality Inspection Institute of Quanzhou, Quanzhou, Fujian, China
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  • Bin Qiu,

    1. Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety (Fuzhou University), Fujian Province Key Laboratory of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou, China
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  • Zhenyu Lin,

    1. Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety (Fuzhou University), Fujian Province Key Laboratory of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou, China
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  • Liyang Shan,

    1. Laboratory of Human Functional, Genomics, Atherosclerosis Research Centre, Nanjing Medical University, Nanjing, China
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  • Lemin Zheng,

    1. The Institute of Cardiovascular Sciences and Institute of Systems Biomedicine, School of Basic Medical Sciences, Peking University Health Science Center, Key Laboratory of Molecular Cardiovascular Sciences of Education Ministry, and Key Laboratory of Cardiovascular Molecular Biology and Regulatory Peptides of Health Ministry, Beijing, China
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  • Jianrong Li,

    1. Food Safety Key laboratory of Zhejiang Province, College of Food Science and Biotechnology, Zhejiang Gongshang University, Hangzhou, China
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    • These authors contributed equally to this work.

  • Guonan Chen

    Corresponding author
    1. Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety (Fuzhou University), Fujian Province Key Laboratory of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou, China
    • Correspondence to: G. N. Chen, Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety (Fuzhou University), Fujian Province Key Laboratory of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou 350002, China.

      E-mail: gnchen@fzu.edu.cn

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    • These authors contributed equally to this work.


Abstract

RATIONALE

A method has been developed for simultaneous determination of the toxins OA, DTX-1, AZA-1, AZA-2 and AZA-3 in various aquatic products as these can cause diarrhoetic shellfish poisoning (DSP) in humans, an intoxication characterized by vomiting and diarrhea.

METHODS

Separation of the toxins was achieved on a C18 column (150 mm × 2.1 mm, 3.5 µm) using an acetonitrile/water gradient with formic acid as an eluent modifier. Electrospray ionisation (ESI) in negative mode was used to generate the molecule related ion [M–H], for OA and DTX-1, while ESI in positive mode was used to generate the molecule related ion [M+H]+ for AZAs. Samples were extracted with 80% methanol, followed by partitioning with ethyl acetate, purified on a Poly-Sery MAX cartridge and finally analyzed by LC/ESI-MS/MS in the multiple reaction monitoring (MRM) mode.

RESULTS

The limit of detection (LOD) and limit of qualification (LOQ) of the method were in the range of 0.02–0.79 µg/kg and 0.07–2.64 µg/kg in Scomberomorus niphonius, blood clam and oyster, respectively, recoveries of the toxins at three fortification levels ranged from 71.3% to 104.8% with relative standard deviation from 1.0% to 12.5%. The calibration curves were well linear between the LC peak area of the selected ion pair and the concentration of the toxins, with the correlation coefficient over 0.99.

CONCLUSIONS

The method was sufficiently sensitive to permit the determination of the toxins DSP and AZA in sea food. Copyright © 2014 John Wiley & Sons, Ltd.

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