腹足纲动物中河豚毒素及其污染物的分析方法优化

Analytical Method Optimization of Tetrodotoxin and Its Contamination in Gastropods.

作者信息

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

机构信息

Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China.

China National Center for Food Safety Risk Assessment, Beijing 100026, China.

出版信息

Foods. 2023 Aug 18;12(16):3103. doi: 10.3390/foods12163103.

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 > 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 (, 565 samples collected in Zhejiang province, China, from 2016 to 2022) were first reported. The detection rate of TTX in 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 .

河豚毒素（TTX）是一种剧毒的海洋生物毒素。本研究开发了一种液相色谱-串联质谱法（LC-MS/MS），结合阳离子交换固相萃取（SPE）净化技术，用于检测腹足类动物中痕量污染和极高含量的TTX。样品基质中的检测限（LOD）为0.5μg/kg。通过筛选出的内标（井冈霉素，IS）进行校准，线性范围为0.1-100 ng/mL（样品基质中为1.5-1500μg/kg），相关系数>0.999。三个加标水平（1.5μg/kg、44μg/kg和1500μg/kg）的平均回收率为82.6-94.4%，相对标准偏差（RSD）小于8.4%。研究了七种腹足类动物（741个样本）中的TTX水平。首次报道了[具体腹足类动物名称未给出]（2016年至2022年在中国浙江省采集的565个样本）中的污染情况和类似物。[具体腹足类动物名称未给出]中TTX的检出率为34.2%。平均浓度为23.1μg/kg，最大值为2327μg/kg。时间分布研究表明，[具体腹足类动物名称未给出]的TTX高污染发生在5月至8月。