Determination of Lipophilic Marine Biotoxins in Shellfish by Online Turbulent Flow Chromatography Coupled to Liquid Chromatography–Tandem Mass Spectrometry

  • Li FangEmail author
  • Fengmei Qiu
  • Xinwei Yu


A novel method based on online turbulent flow chromatography (TFC) combined with liquid chromatography–tandem mass spectrometry (LC–MS/MS) has been established for simultaneous quantitative determination of 11 lipophilic marine toxins (OA, DTX1, DTX2, YTX, hYTX, AZA1, AZA2, AZA3, PTX2, SPX1, and GYM) in shellfish. Sample preparation, including extraction with 75% methanol aqueous solution, centrifugation, and filtration, was followed by online cleanup using TFC. The total run time was within 15.5 min, including online purification, chromatographic separation, and re-equilibration of the TFC system. Various experimental parameters including extraction, purification, separation, and detection were optimized separately in this study. The developed method was validated, and good performance characteristics were obtained. The linear regression coefficients (R2) of matrix-match calibration standard curves established for quantification were higher than 0.9945. The limits of detection and quantification of this method ranged between 0.5 and 4.0, and 1.5 and 10.0 µg/kg, respectively. The average recoveries of spiked target compounds with different concentrations ranged from 80.1 to 113.8%, the intra- and inter-day precision were lower than 12.7% and 14.9%, respectively. The matrix effects were in the range of 76.1–115.9%. The method accuracy was also confirmed with certified reference materials. The results indicate that the developed method has great potential for the routine laboratory analysis or emergency detection of lipophilic marine toxins in shellfish.


Lipophilic marine biotoxins Poisoning Shellfish Turbulent flow chromatography 



This work was financially supported by the Science and Technology Program of Zhoushan (No. 2017B31127); Medical and Health Science and Technology Program of Zhoushan (No. 2017A01).

Conflict of interest

Author Li Fang declares that he has no conflict of interest. Author Feng-mei Qiu declares that she has no conflict of interest. Author Xin-wei Yu declares that he has no conflict of interest

Supplementary material

10337_2019_3705_MOESM1_ESM.doc (126 kb)
Supplementary material 1 (DOC 126 KB)


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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Key Laboratory of Health Risk Factors for Seafood of Zhejiang ProvinceZhoushan Municipal District Center for Disease Control and PreventionZhoushanPeople’s Republic of China
  2. 2.Daishan Center for Disease Control and PreventionDaishanPeople’s Republic of China

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