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

建立超高效液相色谱-串联质谱（UPLC-MS/MS）快速测定水产品中三聚氰胺残留的方法。采用AC-QUITY UPLC BEHHILIC色谱柱（100 mm×2.1 mm,1.7μm）,流动相为乙腈-0.5 mmol/L乙酸铵溶液（0.1%甲酸）,流速为0.3 mL/min。采用电喷雾质谱检测,以正离子模式5 min完成质谱分析。实验结果表明,三聚氰胺在水产品中的检测限为0.05 mg/kg,在0.05-0.50 mg/kg添加水平时的加标回收率为63%-90%,测定结果的相对标准偏差均小于7.2%（n=6）。

The residue of melamine in aquatic product was detected by ultra performance liquid chromatography-tandem mass spectrometer.The sample was extracted and separated on ACQUITY UPLC BEH HILIC column（100 mm×2.1 mm,1.7 μm） with acetonitrile-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 showed that the detection limit was 0.05 mg/kg, and the recoveries ranged from 63% -90% with addtion levels between0. 05 -0.50mg/kg. Relative standard deviations of determination results were less than 7.2% （n =6）.