Simultaneous quantification of Pacific ciguatoxins in fish blood using liquid chromatography–tandem mass spectrometry

Abstract

Ciguatera fish poisoning (CFP) is a food intoxication caused by exposure to ciguatoxins (CTXs) in coral reef fish. Rapid analytical methods have been developed recently to quantify Pacific-CTX-1 (P-CTX-1) in fish muscle, but it is destructive and can cause harm to valuable live coral reef fish. Also fish muscle extract was complex making CTX quantification challenging. Not only P-CTX-1, but also P-CTX-2 and P-CTX-3 could be present in fish, contributing to ciguatoxicity. Therefore, an analytical method for simultaneous quantification of P-CTX-1, P-CTX-2, and P-CTX-3 in whole blood of marketed coral reef fish using sonication, solid-phase extraction (SPE), and liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed. The optimized method gave acceptable recoveries of P-CTXs (74–103 %) in fish blood. Matrix effects (6–26 %) in blood extracts were found to be significantly reduced compared with those in muscle extracts (suppressed by 34–75 % as reported in other studies), thereby minimizing potential for false negative results. The target P-CTXs were detectable in whole blood from four coral reef fish species collected in a CFP-endemic region. Similar trends in total P-CTX levels and patterns of P-CTX composition profiles in blood and muscle of these fish were observed, suggesting a relationship between blood and muscle levels of P-CTXs. This optimized method provides an essential tool for studies of P-CTX pharmacokinetics and pharmacodynamics in fish, which are needed for establishing the use of fish blood as a reliable sample for the assessment and control of CFP.

Chromatograph of P-CTXs in whole blood of wild-caught moray eel

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Acknowledgments

The present work was fully supported by three grants from the Research Grants Council of the Hong Kong Special Administrative Region (CityU3/CRF/08), the National Natural Science Foundation of China (41276110) and a grant from Shenzhen strategic emerging industry development special project, China. We thank Mr. Being Yeeting (Senior Fisheries Scientist, Secretariat of the Pacific Community, New Caledonia) and the Fisheries Division (Ministry of Fisheries and Marine Resource Development, Republic of Kiribati) for facilitating the sample collection. The authors declare they have no competing financial interest.

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Correspondence to Paul K. S. Lam.

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Mak, Y.L., Wu, J.J., Chan, W.H. et al. Simultaneous quantification of Pacific ciguatoxins in fish blood using liquid chromatography–tandem mass spectrometry. Anal Bioanal Chem 405, 3331–3340 (2013). https://doi.org/10.1007/s00216-013-6766-8

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Keywords

  • Ciguatera fish poisoning
  • Pacific ciguatoxins
  • P-CTXs
  • Fish blood
  • LC-MS/MS