阴离子交换固相萃取GC-MS/MS方法检测鱼肉制品中的河豚毒素

Determination of tetrodotoxin in dried fish using anion exchange solid-phase extraction combining with gas chromatography-tandem mass spectrometry

目的建立高灵敏度的检测鱼肉制品中河豚毒素的阴离子交换固相萃取(SPE)气相色谱-串联质谱法。方法采用直接碱解的样品处理方法,将鱼肉制品中的河豚毒素转化为C9碱,经阴离子交换(SAX)固相萃取柱净化、双三甲基硅基三氟乙酰胺(BSTFA)硅烷化衍生后,在气相色谱-串联质谱仪上以选择反应监测(SRM)模式进行检测。结果与结论在最优分析条件下,染毒的鱼肉样品中河豚毒素的线性范围为10～1000μg/kg,检测限为8μg/kg。该方法专属性强、灵敏度高,操作相对简便。

Objective To establish a highly sensitive method for the detection of tetrodotoxin in dried fish using anion exchange solid-phase extraction（SPE） combining with gas chromatography-tandem mass spectrometry.Methods Tetrodotoxin in dried fish was converted directly to C9-base by alkaline hydrolysis and extracted with SAX cartridge column.The C9-base was analyzed after trimethylsilyl derivatization by GC-MS/MS-selected reaction monitoring.Results and Conclusion Under the optimal conditions,the linear calibration curve ranged from 10 to 1000 μg/kg and the limit of detection was 8 μg/kg.The method is highly specific,sensitive and simple.