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高效液相色谱-电喷雾串联质谱法测定鳗鱼中三聚氰胺的残留
邢丽红1, 冷凯良1, 孙伟红1, 谭志军1, 苗钧魁1, 王泽文2
1.中国水产科学研究院黄海水产研究所;2.中国海洋大学
摘要:
建立了利用高效液相色谱-电喷雾串联质谱(LC-MS/MS)法测定鳗鱼(Anguilla japonica)中三聚氰胺残留的方法。采用乙腈和三氯乙酸溶液沉淀蛋白,MCX固相萃取柱净化,提取目标分析物,经SCX-C18均匀混合填装的反相色谱柱分离,选择反应监测(SRM)正离子模式测定。三聚氰胺的定量限为20 μg/kg;在20~500 μg/kg时,峰强度与质量浓度的线性关系良好(r>0.99)。方法的平均回收率为84.82%~91.42%。
关键词:  鳗鱼(anguilla japonica  三聚氰胺  液相色谱路串联质谱仪  残留  测定
DOI:
分类号:
基金项目:国家863计划项目(2008AA100805)
Determinaion of melamine residue in eel using high performance liquid chromatography-electrospray ionization tandem mass spectrometry
XING Li-hong,LENG Kai-liang,SUN Wei-hong,TAN Zhi-jun,MIAO Jun-kui,WANG Ze-wen
Abstract:
The method for the determination of melamine residue in eel using high performance liquid chromatography-electrospray ionization tandem mass spectrometry (LC-MS/MS) was developed. Acetonitril and 1% trichloracetic acid solution was used to precipitate proteins and to dissociate the target analyte from the sample matrix. Then it was degreased and depurated with Oasis MCX solid phase extraction cartridge. A SCX-C18 mixture filled RP-HPLC column was used for separation, and the mass spectrometer was operated in the positive ion mode using select reaction monitoring. The limits of detection was 20 μg/kg for LC-MS/MS. The correlation coefficient of linear calibration curve was over 0.99 within the melamine concentration range 20~500 μg/kg. The average recovery for melamine ranged between 84.82% and 91.42%.
Key words:  eel  melamine  high performance liquid chromatography-electrospray ionization tandem mass spectrometry  residue  determination
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