超高效液相色谱法测定动物源性食品中的三聚氰胺

建立动物源性食品中三聚氰胺含量测定的超高效液相色谱法。鸡蛋样品用1% 三氯乙酸- 乙腈(3:1，V/V)溶液提取、离心、固相萃取柱净化，然后采用CR 色谱柱(阳离子交换填料SCX 与C18 包被型填料按质量比1:4 混合)进行超高效液相色谱分析。兔肉样品用乙腈提取，离心后以强阳离子色谱柱进行超高效液相色谱分析。对色谱条件进行优化，选用236nm 作为检测波长，鸡蛋中三聚氰胺在浓度为1.00～5.00mg/L 的范围内线性关系良好，在添加浓度为1.00、2.00、5.00mg/kg 时，添加回收率在89.24%～91.06% 之间，RSD 小于6.00％。对于兔肉中三聚氰胺浓度在0.4～4mg/L 的范围内线性良好，在添加浓度为2.00、5.00、10.00mg/kg 时，添加回收率在82.65%～86.54% 之间，RSD 小于7.50%。该方法简便、快速，检测灵敏度、准确度及精密度均满足检测要求。

Ultra Performance Liquid Chromatographic Determination of Melamine in Animal-derived Foods

A method for the determination of melamine in animal-derived foods by ultra performance liquid chromatography (UPLC) was established. Egg samples were extracted with a mixture of 1% trichloroacetic acid and acetonitrile (3:1, V/V) and cleaned up using a PCX-SPE column, and the chromatographic separation was achieved on a CR column filled with a mixture of SCX and C18 (1:4, m/m). Melamine in rabbit meat samples was extracted with acetonitrile and injected without clean up into a PAK SCX UG80 column for the chromatographic separation. The detection was performed at UV wavelength of 236 nm. For the analysis using CR column, the calibration curve was linear in the range of 1.00－5.00 mg/L. The average recoveries of melamine in eggs spiked at three levels (1.00, 2.00 and 5.00 mg/kg) were 89.24%－91.06%, with a relative standard deviation less than 6.00%. For the analysis using PAK SCX UG80 column, the calibration curve was linear in the range of 0.4－4 mg/L. The average recoveries in rabbit meat spiked at three levels (2.00, 5.00 and 10.00 mg/kg) were 82.65%－86.54%, with a relative standard deviation less than 7.50%. This method is simple, and its sensitivity, accuracy and prevision all can meet the analytical requirements for melamine.