HPLC-MS法测定鲜鱼中河豚毒素

目的建立用液相色谱-质谱（HPLC-MS）法测定鲜鱼中河豚毒素含量的方法。方法样品经粉碎、酸性水溶液提取、蛋白酶解、石油醚脱脂、有机溶剂甲醇沉淀、固相萃取柱净化后,以液相色谱-质谱法测定,外标法定量。结果鱼肉和鱼肝中河豚毒素在0.10～10 mg/kg范围内呈良好线性关系,相关系数分别为0.9998和0.9991,平均回收率为94.6%~102%,相对标准偏差RSD小于6.6%,方法的最低检出限为0.03 mg/kg。结论该方法操作简便、快速,为饮用水及水产品中河豚毒素的检测、相关的司法鉴定等提供了准确有效的科学依据。

Determination of Tetrodotoxin in Fish by HPLC-MS

Objective To develop a method for the determination of tetrodotoxin in fish by high performance liquid chromatography-mass spectrometry(HPLC-MS).Method After being extracted with acetate acid,hydrolyzed by papain,with fat removed by petroleum ether,precipitated with methanol,and further purified by SPE,samples were analyzed by HPLC-MS and quantified with the external standard method.Results The linear range of tetrodotoxin was 0.10-10 mg/kg in fish meat and liver(R=0.9998 and 0.9991,respectively).The mean recovery was 94.6%~102% and RSD was below 6.6%.The limit of detection was 0.03 mg/kg.Conclusion The established method is simple and efficient.It can provided an accurate and effective approach for the detection of tetrodotoxin in drinking water and fishes in forensic toxicology identification.