超高效液相色谱串联质谱法(UPLC-M/SMS)测定多种食品中三聚氰胺的残留量  

Determination of melamine residue in foods by ultra performance liquid chromatography-electrospray tandem mass spectrometry

作　　者：冯楠[1] 路勇[1] 吴颖[1] 姜洁[1] 谢文东[1] 肖辉[1] 刘丽娟[1] 周新[1] 

机构地区：[1]北京市食品安全监控中心,北京100041

出　　处：《中国卫生检验杂志》2009年第2期248-250,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的：建立多种食品中三聚氰胺残留量的UPLC—MS／MS测定方法和样品前处理方法。方法：样品经l％三氯乙酸溶液提取后，阳离子交换固相萃取柱净化，进行UPLC—MS／MS分析，采用多反应监测模式，外标法定量。采用BEHHILIC色谱柱，以10mmol／L乙酸铵溶液和乙腈为流动相。结果：在50～500μg／kg添加水平范围内，三聚氰胺回收率为76．6％～103．9％，相对标准偏差为6．6％～10．6％，方法测定低限为50μg／kg。结论：方法准确度和稳定性较好，操作简单快捷，样品净化效果好，测定低限能够满足限量要求。Objective：To develop a UPLC - MS/MS method for the determination of melamine residue in foods. Methods：The melamine in samples was extracted with 1% acetocaustin and cleaned up with MCX SPE cartridge, the analyte was determined by UPLC -MS/MS, multi-reaction monitoring （MRM） mode was employed for the quantitative determination, and quantified by the external standard curve. The separation was performed on a UPLC BEH HILIC column with a system of water （ containing 10mmol/L ammonium acetate buffer） - acetonitrile as mobile phase at a flow rate of 0. 3 ml/min. Results ：The limit of determination of this method was 50 μg/kg. The detection limits of 50 - 500μg/kg proved to be much better than the previously reported ones. Average recoveries of melamine ranged from 76. 6% to 103.9%, with relative standard deviations between 6. 6% and 10. 6%. Conclusion：The method is simple, accurate and suitable for the identification and quantification of melamine residue in foods.

关 键 词：UPLC—MS/MS 食品 三聚氰胺 残留 测定 

分 类 号：O657.72[理学—分析化学]