HPLC-MS-ESI法快速测定乳粉及乳制品中三聚氰胺的方法研究

Research on rapid determination of melamine in milk powder and dairy products by HPLC-MS-ESI

目的建立乳粉及乳制品中三聚氰胺含量的HPLC初筛、离子阱质谱确证的测定方法。方法液相色谱以离子对缓冲液∶乙腈=90∶10(V/V)为流动相,Xtimate-C18(4.6 mm×250 mm,5μm)色谱柱,240 nm检测波长,离子阱质谱电离方式:电喷雾电离(ESI),正离子。结果回归方程为:y=1.085 517×104x+8.576 547×104(r2=0.999 925);添加浓度0.8~2.0 mg/kg,回收率82.0%~94.1%,相对标准偏差<5.8%。结论用HPLC进行粗筛,以LC-MS-ESI确证乳粉及乳制品中三聚氰胺的含量,方法简便,重现性好,灵敏度高,定性准确,定量精确。

Objective To establish a determination method of melamine in milk powder and dairy products by HPLC and confirmed by LC-MS.Methods With Xtimate-C 18(4.6 mm×250 mm,5 μm) as chromatographic column,mobile phase of buffer∶acetonitrile =90∶10,PDA and Finnigan LCQ Deca XP MAX MS detector was performed.Results The linear regression function was as follows: y =1.085517×10 4 x +8.576547×10 4(r 2 =0.999925).The average recovery rates were 82.0%～94.1% with added 0.8～2.0 mg/kg,relative standard deviation <5.8%.Concl...