PMID- 37628101 OWN - NLM STAT- PubMed-not-MEDLINE LR - 20230828 IS - 2304-8158 (Print) IS - 2304-8158 (Electronic) IS - 2304-8158 (Linking) VI - 12 IP - 16 DP - 2023 Aug 18 TI - Analytical Method Optimization of Tetrodotoxin and Its Contamination in Gastropods. LID - 10.3390/foods12163103 [doi] LID - 3103 AB - 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 mug/kg. With the calibration of a screened internal standard (validamycin, IS), the linear range was 0.1-100 ng/mL (1.5-1500 mug/kg in sample matrix) with a correlation coefficient of r(2) > 0.999. The average recoveries at three spiking levels (1.5 mug/kg, 44 mug/kg, and 1500 mug/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 mug/kg, and the maximum value was 2327 mug/kg. The time distribution study indicated that high contaminations of TTX occurred from May to August for N. didyma. FAU - Han, Jian-Long AU - Han JL AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China. FAU - Zhang, Lei AU - Zhang L AD - China National Center for Food Safety Risk Assessment, Beijing 100026, China. FAU - Zhou, Ping-Ping AU - Zhou PP AD - China National Center for Food Safety Risk Assessment, Beijing 100026, China. FAU - Xu, Jiao-Jiao AU - Xu JJ AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China. FAU - Pan, Xiao-Dong AU - Pan XD AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China. FAU - Cao, Pei AU - Cao P AD - China National Center for Food Safety Risk Assessment, Beijing 100026, China. FAU - Xu, Xiao-Min AU - Xu XM AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China. LA - eng GR - 2021KY615/Science Research Foundation of Zhejiang Provincial Medicine and Health Program/ PT - Journal Article DEP - 20230818 PL - Switzerland TA - Foods JT - Foods (Basel, Switzerland) JID - 101670569 PMC - PMC10453083 OTO - NOTNLM OT - Neverita didyma OT - cation exchange clean-up OT - gastropods OT - liquid chromatography-tandem mass spectrometry OT - tetrodotoxin COIS- The authors declare no conflict of interest. EDAT- 2023/08/26 10:41 MHDA- 2023/08/26 10:42 PMCR- 2023/08/18 CRDT- 2023/08/26 01:10 PHST- 2023/07/19 00:00 [received] PHST- 2023/08/11 00:00 [revised] PHST- 2023/08/15 00:00 [accepted] PHST- 2023/08/26 10:42 [medline] PHST- 2023/08/26 10:41 [pubmed] PHST- 2023/08/26 01:10 [entrez] PHST- 2023/08/18 00:00 [pmc-release] AID - foods12163103 [pii] AID - foods-12-03103 [pii] AID - 10.3390/foods12163103 [doi] PST - epublish SO - Foods. 2023 Aug 18;12(16):3103. doi: 10.3390/foods12163103.