Analytical Method Optimization of Tetrodotoxin and Its Contamination in Gastropods

oleh: Jian-Long Han, Lei Zhang, Ping-Ping Zhou, Jiao-Jiao Xu, Xiao-Dong Pan, Pei Cao, Xiao-Min Xu

Format: Article
Diterbitkan: MDPI AG 2023-08-01

Deskripsi

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 <i>r</i><sup>2</sup> > 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 <i>Neverita didyma</i> (<i>N. didyma</i>, 565 samples collected in Zhejiang province, China, from 2016 to 2022) were first reported. The detection rate of TTX in <i>N. didyma</i> 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 <i>N. didyma</i>.