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目的本文采用免疫亲和柱选择性吸附样品溶液中的河鲀毒素,建立了测定水产食品中河鲀毒素(TTX)的亲水液相色谱-串联质谱分析方法。方法样品以含1%乙酸的甲醇溶液提取,磷酸盐缓冲溶液稀释,再经免疫亲和柱富集和净化后进样分析。目标物以TSK-gel Amide-80亲水色谱柱(150 mm×2.0 mm,5μm)分离,乙腈-0.1%甲酸水溶液(含5 mmol/L乙酸铵)梯度洗脱,采用电喷雾离子源,选择反应监测(SRM)正离子模式检测,溶剂标准曲线校正,外标法定量。结果 TTX在1~1 000μg/L范围内线性良好,方法的检出限为1μg/kg,定量限为3μg/kg,在3~300μg/kg范围内加标回收率为73.6%~95.2%,相对标准偏差(RSD)为5.37%~10.7%。结论该方法可有效消除复杂基质样品中普遍存在的基质抑制效应,操作简便,色谱保留时间稳定,灵敏度高,准确度和重复性好,适用于烤鱼片、风味鱼干等水产食品中河鲀毒素的测定。
OBJECTIVE To establish a method for the determination of tetrodotoxin (TTX) in aquatic products by liquid chromatography-tandem mass spectrometry (HPLC-MS / MS), using immunoaffinity column for the selective adsorption of tetrodotoxin in the sample solution. Methods The samples were extracted with 1% acetic acid in methanol and diluted with phosphate buffered saline. The samples were analyzed by immunoaffinity column enrichment and purification. The target was separated on a TSK-gel Amide-80 hydrophilic column (150 mm × 2.0 mm, 5 μm) and eluted with a gradient of acetonitrile-0.1% formic acid (containing 5 mmol / L ammonium acetate) using an electrospray ionization source Reaction monitoring (SRM) positive mode detection, solvent calibration curve, external standard quantitative. Results The linearity of TTX in the range of 1 ~ 1000μg / L was good. The detection limit of the method was 1μg / kg, the limit of quantification was 3μg / kg, the recoveries ranged from 73.6% to 95.2% in the range of 3 ~ 300μg / The relative standard deviation (RSD) was 5.37% -10.7%. Conclusion This method can effectively eliminate the matrix inhibition effect that is common in complex matrix samples. The method is simple in operation, stable in chromatographic retention time, high in sensitivity, good in accuracy and repeatability. The method is suitable for fish fillets Determination of toxins.