气相色谱-质谱法测定鸡蛋中三聚氰胺

建立了气相色谱-质谱法测定鸡蛋中三聚氰胺的方法. 鸡蛋样品经三氯乙酸提取,乙酸铅沉淀蛋白后,过MCX阳离子交换固相萃取小柱除去样品基质干扰,用N,O-双三甲基硅基三氟乙酰胺(BSTFA)+三甲基氯硅烷(TMCS)(99+1)衍生,进行气相色谱-质谱分析. 在0.010~2.00 mg/L浓度范围内,线性关系良好(r=0.9996),检出限为0.01 mg/kg. 方法回收率为90.1%~94.7%,RSD为1.7%~5.3%. 方法准确、灵敏,适用于鸡蛋中三聚氰胺的检测.

Determination of Melamine in Eggs by Gas Chromatography-Mass Spectrometry

A gas chromatographic-mass spectrometric method for the quantitative analysis of melamine in eggs has been developed. The sample was extracted by trichloroacetic acid, settled by lead acetate for the protein precipitation, cleaned-up by the MCX cation exchange solid phase extraction column, derivatized with BSTFA+TMCS (99+1) and processed for analysis by the gas chromatography-mass spectrometry. The calibration curves showed good linearity in the range of 0.010~2.00 mg/L for melamine with a correlation coefficent of 0.9996. The limit of detection was 0.01 mg/kg. The recoveries were 90.1%-94.7% and relative standard deviations were 1.7%-5.3%. The method is accurate and sensitive for the determination of melamine in eggs.