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目的针对即食烤鱼片中毒原因分析这一迫切需求,利用亲水液相色谱-串联三重四极杆质谱仪(HILIC-MS/MS)建立了快速定性定量检测即食烤鱼片中河豚毒素的方法。方法取1.0 g即食烤鱼片样品经0.1%甲酸溶液提取,HLB固相萃取柱净化后过膜,亲水液相色谱柱分离,电喷雾离子化,选择反应监测(SRM)模式检测,基质匹配外标法定量。结果在2.5 ng/ml~100 ng/ml时河豚毒素呈现良好的线性关系,相关系数为0.999 5;以3倍基线噪声所对应的浓度为检出限时,即食烤鱼片基质中河豚毒素的方法检出限可达10.0μg/kg;在25μg/kg、100μg/kg和200μg/kg的加标水平时,方法的回收率为73.4%~89.5%,相对标准偏差为2.9%~10.4%。结论该检测方法准确、快速、易操作,能满足即食烤鱼片中河豚毒素的公共卫生应急检测或日常监测要求。
Objective To establish a rapid and qualitative method for the determination of tetrodotoxin in ready-to-eat roasted fillets using the liquid chromatography-tandem triple quadrupole mass spectrometry (HILIC-MS / MS) . Methods The sample of 1.0 g ready-to-eat roasted fish fillet was extracted with 0.1% formic acid solution, purified by HLB solid phase extraction column, separated by hydrophilic liquid chromatography, electrospray ionization, selected reaction monitoring (SRM) External standard method. The results showed good linearity of tetrodotoxin at 2.5 ng / ml ~ 100 ng / ml with a correlation coefficient of 0.999 5. The method of detecting tetrodotoxin in the substrate of roasted fish fillet with the detection limit of 3 times the baseline noise The detection limit was up to 10.0μg / kg. The recoveries were 73.4% -89.5% with relative standard deviations of 2.9% -10.4% at spiked levels of 25μg / kg, 100μg / kg and 200μg / kg. Conclusion The detection method is accurate, rapid and easy to operate, which can meet public health emergency detection or routine monitoring requirements of tetrodotoxin in ready-to-eat roasted fillets.