分子印迹固相萃取-高效液相色谱法同时测定鸡血浆中环丙氨嗪和三聚氰胺残留

Molecularly imprinted solid phase extraction coupled with high performance liquid chromatography for the simultaneous determination of cyromazine and melamine residues in chicken plasma

建立了基于分子印迹固相萃取-高效液相色谱同时测定鸡血浆中环丙氨嗪和三聚氰胺残留方法。以环丙氨嗪为模板分子,甲基丙烯酸为功能单体,合成了对环丙氨嗪和三聚氰胺具有高选择性的分子印迹聚合物。作为固相萃取填料,评价和优化了其分离、富集环丙氨嗪和三聚氰胺的固相萃取条件。血浆用1%三氯乙酸沉淀蛋白,分子印迹固相萃取净化。在辛烷磺酸钠离子对试剂缓冲液(pH 3.0)中,环丙氨嗪和三聚氰胺在240 nm波长处均形成较强紫外吸收峰,实现用离子对反相高效液相色谱紫外同时分析检测。环丙氨嗪和三聚氰胺在0.10～10.0μg/mL范围内线性关系良好,鸡血浆中环丙氨嗪和三聚氰胺的回收率均高于70%,RSD<10%,检出限达0.05μg/mL。

A high performance liquid chromatographic method based on molecularly imprinted solid-phase extraction for the simultaneous determination of cyromazine（CYR） and melamine（MEL） residues in chicken plasma was developed.Molecularly imprinted polymers with high selectivity to CYR and MEL were prepared using CYR as a template,methacrylic acid as monomer,ethylene glycol dimethacrylate as cross-linker.The characteristics and solid phase extraction conditions of the molecularly imprinted polymers as adsorptive material for the selective extraction and enrichment of CYR and MEL were evaluated.The plasma sample was precipitated by 1% trichloroacetic acid solution,further cleaned up using the molecularly imprinted solid-phase extraction cartridge.An obvious ultraviolet absorbance at wavelength of 240 nm was observed when CYR and MEL were in the system of sodium octanesulfonate（pH 3.0） buffer-acetonitrile（82：18,V/V）.Therefore,the two analytes were determined by ion-pair reversed phase HPLC.The method had good linearity in the range of 0.10-10.0 μg/mL for two anayltes.The obtained recoveries were above 70% with the relative standard deviations of less than 10% for both CYR and MEL.The limits of detection of CYR and MEL in chicken plasma were ca.0.05 μg/mL.