色谱2012，Vol.30Issue(7)：677-683,7.DOI:10.3724/SP.J.1123.2012.01021
固相萃取-亲水相互作用色谱/串联质谱法同时测定食品中三聚氰胺和三聚氰酸
Simultaneous determination of melamine and cyanuric acid in foodstuffs by solid phase extraction-hydrophilic interaction chromatography-tandem mass spectrometry
摘要
Abstract
A method based on solid phase extraction-liquid chromatography-tandem mass spectrometry ( LC-MS/MS) for the simultaneous determination of melamine and cyanuric acid in foodstuffs is presented. The melamine and cyanuric acid residues were extracted by acetonitrile and water, degreased by hexane, and the extract was cleaned-up by a mixed-mode solid phase-extraction column (MCT) of hydrophilic functional silica gel sorbent and cation exchange resin. The LC separation was performed on a hydrophilic interaction chromatograph, the melamine and cyanuric acid were determined by MS/MS in positive-negative switched electrospray ionization mode, multiple reaction monitoring (MRM) mode, and quantified by isotope internal standard method. The melamine and cyanuric acid were linear in the range of 10 - 2 500μg/L with the correlation coefficients (r) higher than 0. 99, and the limits of quantification were 25 (jig/kg and 50μg/kg, respectively. The recoveries of melamine and cyanuric acid spiked in animal-derived foods, plant-derived foods, milk and milk products were in the range of 70. 0% -129.6% and 70.0% - 128.6%, respectively, with the relative standard deviations (RSD) of 1.4%- 23. 3% and 2. 8% - 18. 7%, respectively. The method can meet the requirement for the determination of melamine and cyanuric acid in foodstuffs simultaneously.关键词
固相萃取/液相色谱/串联质谱/三聚氰胺/三聚氰酸/食品Key words
solid phase extraction (SPE)/liquid chromatography-tandem mass spectrometry(LC-MS/MS)/melamine/cyanuric acid/foodstuffs分类
化学化工引用本文复制引用
赵善贞,邓晓军,伊雄海,韩丽,盛永刚,张晓梅,吴巧彬..固相萃取-亲水相互作用色谱/串联质谱法同时测定食品中三聚氰胺和三聚氰酸[J].色谱,2012,30(7):677-683,7.基金项目
上海市技术贸易措施应对专项(09TBT005). （09TBT005）
