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Optimization of simultaneous analysis of tetrodotoxin, 4-epitetrodotoxin, 4,9-anhydrotetrodotoxin, and 5,6,11-trideoxytetrodotoxin by hydrophilic interaction liquid chromatography–tandem mass spectrometry

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Abstract

Recently, liquid chromatography–mass spectrometry (LC–MS) has been recognized as a useful method to analyze tetrodotoxin (TTX), the primary toxin for puffer fish poisoning. TTX usually exists with its chemically interchangeable analogs, such as 4-epiTTX and 4, 9-anhydroTTX. TTX and 4-epiTTX have the same molecular weight and the same fragmentation pattern by tandem mass spectrometry (MS–MS). In this study, we optimized conditions for hydrophilic interaction liquid chromatography (HILC)–MS–MS to quantitate TTX, 4-epiTTX, 4,9-anhydroTTX, and 5,6,11-trideoxyTTX with good separation. The relationships between the applied amounts of each TTX analog to the HILC–MS–MS instrument and the peak areas showed good linearity in the ranges examined. The lower limits of detection (signal-to-noise ratio = 3) were 64 pg on-column for TTX, 128 pg for both 4-epiTTX and 4,9-anhydroTTX, and 180 pg for 5,6,11-trideoxyTTX using an API 2000 mass spectrometer.

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Acknowledgments

This work was supported by a Grant-in Aid for Scientific Research from the Japan Society for the Promotion of Science (No. 21380070). The authors thank Prof. Teruo Miyazawa, Tohoku University, Sendai, Japan, for the opportunity to use the 4000QTRAP instrument.

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Correspondence to Mari Yotsu-Yamashita.

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Yotsu-Yamashita, M., Jang, JH., Cho, Y. et al. Optimization of simultaneous analysis of tetrodotoxin, 4-epitetrodotoxin, 4,9-anhydrotetrodotoxin, and 5,6,11-trideoxytetrodotoxin by hydrophilic interaction liquid chromatography–tandem mass spectrometry. Forensic Toxicol 29, 61–64 (2011). https://doi.org/10.1007/s11419-010-0106-x

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  • DOI: https://doi.org/10.1007/s11419-010-0106-x

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