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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 high sensitivity anion exchange liquid phase extraction (SPE) gas chromatography-tandem mass spectrometry for the detection of tetrodotoxin in fish products. Methods Direct alkali hydrolysis was used to convert tetrodotoxin in fish products to C9 base, purified by anion exchange (SAX) solid phase extraction column and silylated with bistrimethylsilyl trifluoroacetamide (BSTFA) After that, it was detected by selective reaction monitoring (SRM) mode on a gas chromatography-tandem mass spectrometer. RESULTS AND CONCLUSION Under the optimal analytical conditions, the linear range of tetrodotoxin in fish samples was 10 ~ 1000μg / kg and the detection limit was 8μg / kg. The method is highly specific, high sensitivity and relatively easy to operate.