超高效液相色谱-串联质谱法测定水产品中三聚氰胺残留量

Determination of Melamine Residues in aquatic products by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

本文建立超高效液相色谱一串联质谱（UPLC—MS／MS）快速测定水产品中三聚氰胺残留的方法。色谱条件：ACQUITYUPLCBEHHILIC柱（2．1×100mill，1.7m），流动相：乙腈-0．5mmol／L酸铵溶液（0．1％甲酸），流速：0．3mL／min。采用电喷雾质谱检测，以正离子模式5min就完成了质谱分析。实验结果表明，三聚氰胺在水产品中的检测限为0．05mg／kg，在0．05—0．50mg／kg添加水平时加标回收率为63％-90％之间，相对标准偏差（RSD，n=6）均小于7．2％。

The residue of melamine in aquatic product was studied by ultra performance liquid chromatography-tandem mass spectrometer. The sample was extracted and separated on ACQUITY UPLC BEH HILIC column （2.1 × 100 mm, 1.Tin） with acelonitrile-0.5 mmol./L ammonium acetate （0.1% formic acid） as the mobile phase at flow rate 0.3 mL/min. The detection was performed by tandem mass spectrometry, with electrospray ionization in positive mode （ES＋） in five minutes. Experimental results shoowed that the limit of detection was 0.05 mg/kg, the recoveries between 0.05-0.50 mg/kg levels ranged from 63% to 90%. Relative standard deviations （n=6） were less than 7.2% .