上海海洋大学学报2012，Vol.21Issue(6)：1058-1063,6.
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)
摘要
Abstract
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Key words
tetrodotoxin/C9-base/solid phase extraction/gas chromatography-mass spectrometry分类
化学化工引用本文复制引用
黄清发,孙振中,戚隽渊,孙建华,黄德凤,张玉平,刘琴..河鲀毒素固相萃取-气相色谱-质谱法研究[J].上海海洋大学学报,2012,21(6):1058-1063,6.基金项目
养殖河鲀鱼毒性检测技术研究[沪农科攻字（2010）第2-6号] （）
