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10.3390/foods12163103
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Article

Analytical Method Optimization of Tetrodotoxin and Its Contamination in Gastropods

by
Jian-Long Han
1,
Lei Zhang
2,
Ping-Ping Zhou
2,
Jiao-Jiao Xu
1,
Xiao-Dong Pan
1,
Pei Cao
2,* and
Xiao-Min Xu
1,*
1
Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China
2
China National Center for Food Safety Risk Assessment, Beijing 100026, China
*
Authors to whom correspondence should be addressed.
Foods 2023, 12(16), 3103; https://doi.org/10.3390/foods12163103
Submission received: 19 July 2023 / Revised: 11 August 2023 / Accepted: 15 August 2023 / Published: 18 August 2023
(This article belongs to the Special Issue Contaminants in Seafood: Prevention, Control, and Detection)
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Abstract

Tetrodotoxin (TTX) is an extremely potent marine biotoxin. An analytical method was developed for both trace contamination and extremely high levels of TTX in gastropods by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with clean-up of cation exchange solid phase extraction (SPE) in this study. The limit of detection (LOD) in the sample matrix was 0.5 μg/kg. With the calibration of a screened internal standard (validamycin, IS), the linear range was 0.1–100 ng/mL (1.5–1500 μg/kg in sample matrix) with a correlation coefficient of r2 > 0.999. The average recoveries at three spiking levels (1.5 μg/kg, 44 μg/kg, and 1500 μg/kg) were 82.6–94.4% with relative standard deviations (RSDs) less than 8.4%. TTX levels in seven gastropods (741 samples) were studied. The contamination and analogues in Neverita didyma (N. didyma, 565 samples collected in Zhejiang province, China, from 2016 to 2022) were first reported. The detection rate of TTX in N. didyma was 34.2%. The average concentration was 23.1 μg/kg, and the maximum value was 2327 μg/kg. The time distribution study indicated that high contaminations of TTX occurred from May to August for N. didyma.
Keywords: tetrodotoxin; gastropods; Neverita didyma; cation exchange clean-up; liquid chromatography-tandem mass spectrometry tetrodotoxin; gastropods; Neverita didyma; cation exchange clean-up; liquid chromatography-tandem mass spectrometry

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MDPI and ACS Style

Han, J.-L.; Zhang, L.; Zhou, P.-P.; Xu, J.-J.; Pan, X.-D.; Cao, P.; Xu, X.-M. Analytical Method Optimization of Tetrodotoxin and Its Contamination in Gastropods. Foods 2023, 12, 3103. https://doi.org/10.3390/foods12163103

AMA Style

Han J-L, Zhang L, Zhou P-P, Xu J-J, Pan X-D, Cao P, Xu X-M. Analytical Method Optimization of Tetrodotoxin and Its Contamination in Gastropods. Foods. 2023; 12(16):3103. https://doi.org/10.3390/foods12163103

Chicago/Turabian Style

Han, Jian-Long, Lei Zhang, Ping-Ping Zhou, Jiao-Jiao Xu, Xiao-Dong Pan, Pei Cao, and Xiao-Min Xu. 2023. "Analytical Method Optimization of Tetrodotoxin and Its Contamination in Gastropods" Foods 12, no. 16: 3103. https://doi.org/10.3390/foods12163103

APA Style

Han, J.-L., Zhang, L., Zhou, P.-P., Xu, J.-J., Pan, X.-D., Cao, P., & Xu, X.-M. (2023). Analytical Method Optimization of Tetrodotoxin and Its Contamination in Gastropods. Foods, 12(16), 3103. https://doi.org/10.3390/foods12163103

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