河豚鱼肝脏中河豚毒素超高效液相色谱-三重四极杆质谱快速检测  

Rapid determination of tetrodotoxin in puffer fish liver by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry

作　　者：郭境颖 张锦宏 蔡茂荣[1] 陈锦钟 林巧妹[1] 李海杰 GUO Jing-ying;ZHANG Jin-hong;CAI Mao-rong;CHEN Jin-zhong;LIN Qiao-mei;LI Hai-jie(Zhangzhou Municipal Center for Disease Control and Prevention,Zhangzhou,Fujian 363007,China)

机构地区：[1]漳州市疾病预防控制中心,福建漳州363007

出　　处：《中国卫生检验杂志》2022年第17期2057-2060,共4页Chinese Journal of Health Laboratory Technology

基　　金：漳州市科学技术局自然科学基金(ZZ2020J14);福建省卫健委医学创新课题(2020CXB040)。

摘　　要：目的建立实验室河豚鱼肝脏中河豚毒素(TTX)超高效液相色谱-三重四极杆质谱联用技术快速检测方法。方法参照GB 5009.206—2016(第二法),简化河豚鱼肝脏样品前处理的提取、净化操作步骤及采用全基质标准曲线校正法定量。结果样品经0.1%乙酸水溶液提取后、置于沸水浴中加热10 min、超声提取15 min,12000 r/min离心5 min,HLB柱净化,在1μg/L~500μg/L线性关系良好(r^(2)=0.9991),方法检出限为1.5μg/L,定量限为5.0μg/L;添加质量浓度为50μg/kg、100μg/kg、200μg/kg,平均回收率分别为75.7%、85.2%和81.4%,相对标准偏差分别为3.9%、3.6%和2.8%;同GB 5009.206—2016(第二法)比较,样品前处理耗材成本降低88.71%、检测效率提高了4.0倍。结论本方法结果可靠、快捷、简便、灵敏、成本低,符合GB/T 27404—2008的方法确认技术要求,检出限满足于“农办渔[2016]53号”规定的2.2 mg/kg(以鲜品计)限量指标要求,适用于河豚鱼肝中TTX的检测。Objective To establish a rapid detection method for tetrodotoxin(TTX)in puffer fish liver by ultra-performance liquid chromatography-triple quadrupole mass spectrometry.Methods According to GB 5009.206—2016(the second method),the extraction and purification procedures of puffer fish liver sample pre-treatment were simplified,and the whole matrix standard curve correction method was adopted for quantitative analysis.Results The samples were extracted with 0.1%acetic acid aqueous solution,heated in boiling water bath for 10 min,then extracted with ultrasonic for 15 min,centrifuged at12000 r/min for 5 min,and finally purified by HLB column.The results showed a good linear relationship in the range of1μg/L-500μg/L(r^(2)=0.9991).The limit of detection was 1.5μg/L and the limit of quantification was 5.0μg/L.Under the spiked levels of 50μg/kg,100μg/kg,200μg/kg,the average recoveries were 75.7%,85.2%,and 81.4%,respectively,with the relative standard derivations(RSDs)of 3.9%,3.6%,and 2.8%,respectively.Compared with GB 5009.206—2016(the second method),the cost of sample pre-treatment consumables in this method is reduced by 88.71%and the detection efficiency is improved by 4.0 times.Conclusion The method is reliable,rapid,simple,sensitive and low-cost,and meets the technical requirements of GB/T 27404—2008.Besides,the detection limit of this method can meet the requirements of 2.2 mg/kg(fresh product),which is stipulated in Agricultural Fishery[2016]No.53.Therefore,this method is suitable for the detection of TTX in puffer fish liver.

关 键 词：河豚鱼 河豚毒素 超高效液相色谱-三重四极杆质谱法 快速检测 

分 类 号：O657.63[理学—分析化学]