DSPE-HPLC-MS法测定水产品中的三聚氰胺

Determination of melamine in aquatic products by high performance liquid chromatography-mass spectrometry with dispersive solid phase extraction

建立分散固相萃取-高效液相色谱质谱联用法测定水产品中三聚氰胺的方法。样品用甲醇、pH 4.5的乙酸铵缓冲溶液提取,分散固相萃取净化。经Thermo Fisher Hyper-sil Gold C18柱(150mm×2.1mm,5μm)分离,选择反应监测(SRM)正离子模式测定。结果表明,三聚氰胺含量为5～50ng/mL时线性关系良好,其线性方程为Y=8 958.7 X-3 327.8,相关系数R2=0.999 6,检出限为0.01mg/kg,平均回收率在82.8%～100.4%,RSD均小于5.0%。

A method for determination of melamine in aquatic products was established by high performance liquid chromatography-mass spectrometry（HPLC-MS）.Samples were extracted with Methanol,in pH 4.5 by buffer solution of ammonium,and then cleaned with dispersive solid phase extraction.After extracted and separated on a Thermo Fisher Hypersil Gold C18（150 mm× 2.1 mm,5 μm）, the analytes were detected by HPLC-MS with the selected reaction monitoring（SRM） mode.The calibration curves of melamine were linear in the range of 5 ng/mL^50 ng/mL form,the linear equation was Y = 8 958.7 X-3 327.8, the correlation coefficient was 0.999 6,the limit of quantization was 0.01 mg/kg,and the average recovery was in the range of 82.8% ~ 100.4%,RSD〈5.0%.