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目的:建立一种高效液相色谱-电喷雾串联质谱法测定鱼类中雪卡毒素P-CTX1含量的方法。方法:鱼类样品经丙酮提取后,用冷冻脱脂,经PSA氨基柱净化,以乙腈-水作为流动相,在Atlantis色谱柱(150 mm×2.1 mm×5μm)上,梯度改变乙腈在流动相中的比例和流速,采用HPLC/MS/MS电喷雾电离(ES-I),阳离子模式,多反应监测(MRM)方式检测,外标法定量。结果:雪卡毒素在鱼肉中的含量范围为0.5μg/L～20μg/L时,线性关系良好(r=0.9998)。在0.5 ng/kg、2.0 ng/kg和10.0 ng/kg添加水平范围内的平均回收率为88%~94%,相对标准偏差小于8.6%,方法的检出限为1.0 ng/kg。结论:本法简便快速,精密度较高,重现性较好,对鱼类中痕量雪卡毒素具有良好的分析鉴定效果。
Objective: To establish a method for the determination of P-CTX1 in fish by high performance liquid chromatography-electrospray ionization tandem mass spectrometry. Methods: The samples of fish were extracted with acetone, degreased by freezing, purified by PSA column, acetonitrile-water was used as the mobile phase, and the gradient of acetonitrile on the Atlantis column (150 mm × 2.1 mm × 5 μm) The ratio and flow rate were determined by HPLC / MS / MS electrospray ionization (ES-I), cation mode and multi-reaction monitoring (MRM). Results: The linear range of cicliotoxin in fish was 0.5μg / L ~ 20μg / L (r = 0.9998). The average recovery within the range of 0.5 ng / kg, 2.0 ng / kg and 10.0 ng / kg was 88% ~ 94% with the relative standard deviation less than 8.6%. The detection limit was 1.0 ng / kg. Conclusion: This method is simple, rapid, accurate and reproducible. It has good analytical and identification results for trace amounts of ciguatoxin in fish.