超高效液相色谱-电喷雾串联质谱法测定河豚鱼干中的河豚毒素

Determination of Tetrodotoxin in Dried Puffer Fish Product by Ultra High Performance Liquid Chromatography-tandem Mass Spectrometry

目的建立了超高效液相色谱-电喷雾串联质谱法（UPLC-ESI-MS/MS）测定河豚鱼干中河豚毒素的方法。方法以河豚鱼干为原料,样品在100℃用1%乙酸（V/V）溶液超声提取,C18固相萃取柱除杂净化后,以乙腈-0.1%甲酸水为流动相,经AtlantisTM HILIC Silica（3μm,150mm×2.1mm）色谱柱分离,采用多重反应监测（MRM）正离子模式进行检测,用LC/MS/MS外标法定量。结果该方法在1.00~100.00μg/L范围内呈线性关系;定量限（LOQ）为0.01mg/kg;3个添加水平的平均回收率83.7%~89.8%,RSD为3.6%~4.3%。结论该方法简便快速、灵敏度高,适用于河豚鱼干制品中河豚毒素的检测。

Objective To establish a method of ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-ESI-MS/MS）for the detection of tetrodotoxin in dried puffer fish products. Methods Multiple dried puffer fish products were extracted with 1% acetic acid（V/V）,purified by C18solid-phase extraction cartridges.The objective compounds were separated using AtlantisTM HILIC Silica column（3μm,150mm×2.1mm）with acetonitrile-water（0.1%formic acid）as mobile phase and analyzed by mass spectrometry in the positive electrospray ionization under multiple monitoring mode（MRM）,and then detected by LC/MS/MS with external standard method. Results The LOQ for TTX was 0.01mg/kg,the average recoveries were from 83.7%to 89.8% at the spiked level of 1.0-100μg/L with the relative standard deviation of 3.6%-4.3%. Conclusion The method is simple,rapid,sensitive and suitable for the determination of tetrodotoxin in dried puffer fish products.