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目的建立准确、快速检测河鲀毒素(tetrodotoxin,TTX)的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)的分析方法,了解市售烤鱼片、鱿鱼干制品和鱼丸中河鲀毒素污染状况。方法样品经2%乙酸/甲醇溶液超声离心提取后,通过MCX固相萃取柱进行净化处理,采用液相色谱串联质谱法进行检测。结果市售的107份样品中,鱿鱼干制品和鱼丸中没有检出TTX;64份烤鱼片样品中检出16份含有TTX,检出率为25.0%。结论部分烤鱼片中TTX呈阳性,建议生产厂家严把原料关,监管部门应加强对市售烤鱼片标签标识的监管。
OBJECTIVE To establish an accurate and rapid detection method for tetrodotoxin (TTX) by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) Squid dried fish products and fish poisoning contaminants. Methods The samples were centrifuged by 2% acetic acid / methanol solution and purified by MCX solid phase extraction column. The samples were detected by LC-MS / MS. Results Among the 107 commercially available samples, no TTX was detected in the dried squid and fish balls; 16 out of 64 roasted fish samples contained TTX and the detection rate was 25.0%. Conclusion Some of the roasted fish fillets are positive for TTX. It is recommended that the manufacturer strictly control the raw materials, and the regulatory authorities should strengthen the supervision on the labeling of the labeled fish on the market.