河鲀毒素固相萃取-气相色谱-质谱法研究  

A method to determine tetrodotoxin (TTX) in globefish by solid-phase extractions and gas chromatography-mass spectrometry(GC-MS)

作　　者：黄清发[1] 孙振中[1] 戚隽渊[1] 孙建华[1] 黄德凤[1] 张玉平[1] 刘琴[1] 

机构地区：[1]上海市水产研究所,上海200433

出　　处：《上海海洋大学学报》2012年第6期1058-1063,共6页Journal of Shanghai Ocean University

基　　金：养殖河鲀鱼毒性检测技术研究[沪农科攻字(2010)第2-6号]

摘　　要：建立了固相萃取-气相色谱-质谱法测定河鲀鱼中河鲀毒素的分析方法。河鲀鱼肉用2%乙酸甲醇溶液提取出河鲀毒素,石油醚脱脂,浓缩蒸干,然后用强碱将河鲀毒素水解成2-氨基-8-羟基-6-羟甲基-喹唑啉(C9生物碱),水解液经过MCX阳离子交换固相萃取柱净化、BSTFA衍生,采用气相色谱-质谱法全扫描方式定性分析,定性离子376,392,407,选择离子扫描方式定量分析,定量离子392。河鲀毒素在0.05～5.0μg/mL范围内具有良好的线性,相关系数R2=0.997 5,样品添加浓度为0.02、0.10、0.50mg/kg,测定6次,方法回收率为64.0%～92.8%,相对标准偏差RSD为5.41%～8.63%,方法检测限为5.0μg/kg。实验结果表明,建立的固相萃取-气相色谱-质谱法方法灵敏度高,净化效果好,定性、定量准确。A method to determine tetrodotoxin（TTX） in globefish by solid-phase extractions and gas chromatography-mass spectrometry（GC-MS） is described.TTX in globefish sample was extracted with 2% acetic acid/methanol,defatted by petroleum ether,evaporated to dryness under reduced pressure.Then the compound was converted to 2-amino-6-hydroxymethyl-8-hydroxyquinazoline（C9-base） under alkaline conditions and extracted by use of an MCX extraction cartridge.The C9-base was analyzed after trimethylsilyl derivation（TMS） C9-base by GC-MS-scan mode,the qualified ions are 376,392,407.（TMS） C9-base is quantified by GC-MS-selected ion monitoring.The quantified ion was 392.The calibration curve was linear in the range of 0.05-5.0 μg /mL and linear relationship R2=0.997 5.For the 0.02,0.1,0.5 mg/kg spiked samples,the recovery rate were 64.0%-92.8%,RSDs were 5.41%-8.63% for six times,and the limitation of quantification was 5.0 μg/kg.From the results of above,detection of TTX in aquatic products by solid-phase extractions and gas chromatography/mass spectrometry（GC-MS） is sensitive,accurate and feasible.

关 键 词：河鲀毒素 C9生物碱 固相萃取 气相色谱-质谱法 

分 类 号：O653.63[理学—分析化学]