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 X 2.1 mm, 5祄), the analytes were detected by HPLC桵S with the selected reaction monitoringt SRM) mode. The calibration curves of melamine were linear in the range of 5 ng/mL~50 ng/mL form, the linear e-quation was Y = 8 958.7 X ? 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%. RSCX5. 0%.%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、pH4.5的乙酸铵缓冲溶液提取,分散固相萃取净化.经Thermo Fisher Hypersil Gold C18柱(150 mm×2.1 mm,5 μm)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5～50 ng/mL时线性关系良好,其线性方程为y=8 958.7X-3 327.8,相关系数R2=0.999 6,检出限为0.01 mg/kg,平均回收率在82.8％～100.4％,RSD均小于5.0％.
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