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Validation of an accelerated solvent extraction liquid chromatography–tandem mass spectrometry method for Pacific ciguatoxin-1 in fish flesh and comparison with the mouse neuroblastoma assay

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Abstract

Ciguatera fish poisoning (CFP) is a global foodborne illness caused by consumption of seafood containing ciguatoxins (CTXs) originating from dinoflagellates such as Gambierdiscus toxicus. P-CTX-1 has been suggested to be the most toxic CTX, causing ciguatera at 0.1 μg/kg in the flesh of carnivorous fish. CTXs are structurally complex and difficult to quantify, but there is a need for analytical methods for CFP toxins in coral reef fishes to protect human health. In this paper, we describe a sensitive and rapid extraction method using accelerated solvent extraction combined with high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS) for the detection and quantification of P-CTX-1 in fish flesh. By the use of a more sensitive MS system (5500 QTRAP), the validated method has a limit of quantification (LOQ) of 0.01 μg/kg, linearity correlation coefficients above 0.99 for both solvent- and matrix-based standard solutions as well as matrix spike recoveries ranging from 49% to 85% in 17 coral reef fish species. Compared with previous methods, this method has better overall recovery, extraction efficiency and LOQ. Fish flesh from 12 blue-spotted groupers (Cephalopholis argus) was assessed for the presence of CTXs using HPLC-MS/MS analysis and the commonly used mouse neuroblastoma assay, and the results of the two methods were strongly correlated. This method is capable of detecting low concentrations of P-CTX-1 in fish at levels that are relevant to human health, making it suitable for monitoring of suspected ciguateric fish both in the environment and in the marketplace.

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References

  1. Lewis RJ (2006) Toxicon 48:799–809

    Article  CAS  Google Scholar 

  2. Gillespie NC, Lewis RJ, Pearn JH, Bourke AT, Holmes MJ, Bourke JB, Shields WJ (1986) Med J Aust 145:584–590

    CAS  Google Scholar 

  3. Yasumoto T, Nakajima I, Bagnis R, Adachi R (1977) Bull Jpn Soc Sci Fish 43:1021–1026

    Google Scholar 

  4. Lewis RJ, Holmes MJ (1993) Comp Biochem Physiol C 106:615–628

    CAS  Google Scholar 

  5. Pottier I, Vernoux JP, Jones A, Lewis RJ (2002) Food Addit Contam 19:1034–1042

    Article  CAS  Google Scholar 

  6. Murata M, Legrand AM, Ishibashi Y, Fukui M, Yasumoto T (1990) J Am Chem Soc 112:4380–4386

    Article  CAS  Google Scholar 

  7. Juranovic LR, Park DL (1991) Rev Environ Contam Toxicol 117:51–94

    CAS  Google Scholar 

  8. Lehane L, Lewis RJ (2000) Int J Food Microbiol 61:91–125

    Article  CAS  Google Scholar 

  9. Hokama Y, Banner AH, Boylan DB (1977) Toxicon 15:317–325

    Article  CAS  Google Scholar 

  10. Hokama Y, Takenaka WE, Nishimura KL, Ebesu JS, Bourke R, Sullivan PK (1998) J AOAC Int 81:727–735

    CAS  Google Scholar 

  11. Campora CE, Hokama Y, Yabusaki K, Isobe M (2008) J Clin Lab Anal 22:239–245

    Article  CAS  Google Scholar 

  12. Manger RL, Leja LS, Lee SY, Hungerford JM, Hokama Y, Dickey RW, Granade HR, Lewis R, Yasumoto T, Wekell MM (1995) J AOAC Int 78:521–527

    CAS  Google Scholar 

  13. Lewis RJ, Jones A, Vernoux JP (1999) Anal Chem 71:247–250

    Article  CAS  Google Scholar 

  14. Lewis RJ, Yang AJ, Jones A (2009) Toxicon 54:62–66

    Article  CAS  Google Scholar 

  15. Lewis RJ, Sellin M (1992) Toxicon 30:915–919

    Article  CAS  Google Scholar 

  16. Stewart I, Eaglesham GK, Poole S, Graham G, Paulo C, Wickramasinghe W, Sadler R, Shaw GR (2010) Toxicon 56:804–812

    Article  CAS  Google Scholar 

  17. Carabias-Martinez R, Rodriguez-Gonzalo E, Revilla-Ruiz P, Hernandez-Mendez J (2005) J Chromatogr A 1089:1–17

    Article  CAS  Google Scholar 

  18. Lewis RJ, Sellin M, Poli MA, Norton RS, MacLeod JK, Sheil MM (1991) Toxicon 29:1115–1127

    Article  CAS  Google Scholar 

  19. Hamilton B, Hurbungs M, Vernoux JP, Jones A, Lewis RJ (2002) Toxicon 40:685–693

    Article  CAS  Google Scholar 

  20. Wong CK, Hung P, Lee KLH, Kam KM (2005) Toxicon 46:563–571

    Article  CAS  Google Scholar 

  21. Draisci R, Marchiafava C, Palleschi L, Cammarata P, Cavalli S (2001) J Chromatogr B Biomed Sci Appl 753:217–223

    Article  CAS  Google Scholar 

  22. Poerschmann J, Trommler U, Biedermann W, Truyen U, Lucker E (2006) J Chromatogr A 1127:26–33

    Article  CAS  Google Scholar 

  23. Poerschmann J, Carlson R (2006) J Chromatogr A 1127:18–25

    Article  CAS  Google Scholar 

  24. Dechraoui MYB, Tiedeken JA, Persad R, Wang ZH, Granade HR, Dickey RW, Ramsdell JS (2005) Toxicon 46:261–270

    Article  CAS  Google Scholar 

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Acknowledgements

We thank Ms. Rachel P. P. Wong (School of Biological Science, The University of Hong Kong) for identification of fish species and Asia Pacific Application Support Center of AB Sciex for providing 5500 QTRAP and technical assistance. The work described in this paper was fully supported by a grant from the Research Grants Council of the Hong Kong Special Administrative Region, China (CityU3/CRF/08).

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Authors and Affiliations

  1. State Key Laboratory in Marine Pollution and Department of Biology and Chemistry, City University of Hong Kong, Tat Chee Avenue, Kowloon, Hong Kong SAR, China

    Jia Jun Wu, Yim Ling Mak, Margaret B. Murphy, Wing Hei Chan & Paul K. S. Lam

  2. State Key Laboratory in Marine Pollution and Department of Biology and Chemistry, City University of Hong Kong, Tat Chee Avenue, Kowloon, Hong Kong SAR, China

    James C. W. Lam & Leo L. Chan

  3. School of Biological Sciences, The University of Hong Kong, Pokfulam Road, Hong Kong, Hong Kong SAR, China

    Mingfu Wang

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  1. Jia Jun Wu
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  2. Yim Ling Mak
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Correspondence to Paul K. S. Lam.

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Wu, J.J., Mak, Y.L., Murphy, M.B. et al. Validation of an accelerated solvent extraction liquid chromatography–tandem mass spectrometry method for Pacific ciguatoxin-1 in fish flesh and comparison with the mouse neuroblastoma assay. Anal Bioanal Chem 400, 3165–3175 (2011). https://doi.org/10.1007/s00216-011-4977-4

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  • DOI: https://doi.org/10.1007/s00216-011-4977-4

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