超高效液相色谱-串联质谱法检测河鲀毒素

Determination of tetrodotoxin by ultra performance liquid chromatography-tandem mass spectrometry

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 a method for determination of tetrodotoxin (TTX) by ultra performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS) and to elucidate the contamination situation of TTX in grilled fillet, shredded squid and fish ball.MethodsTTX was extracted from samples by 2% acetic acid-methanol, and then purified by solid-phase extraction with MCX. The samples were detected by liquid chromatography-tandem mass spectrometry.Results TTX was not detected in shredded squid and fish ball. Sixteen grilled fillet samples were detected TTX and the detection rate was 25.0%. Conclusion TTX is detected in some grilled fillet. The raw materials should be strictly controlled by manufacturers and the regulatory authorities should increase the regulation standards for the grilled fillet products.