基质固相分散-气相色谱-串联质谱法测定焙烤食品中氨基甲酸乙酯

Determination of ethyl carbamate in baking foods by matrix solid phase dispersion and gas chromatography tandem mass spectrometry

建立了焙烤食品中氨基甲酸乙酯的基质固相分散-气相色谱-串联质谱联用(MSPD-GC/MS/MS)的测定方法,样品经硅藻土吸附后转入层析柱中进行基质固相分散萃取,用正己烷洗脱非极性成分,再用二氯甲烷洗脱目标物,采用DB-225MS毛细管柱分离样品,气相色谱-串联质谱法测定氨基甲酸乙酯的含量。结果表明,该方法标准曲线线性良好,线性范围为5～500μg/L,相关系数r=0.9997,方法检出限2.5μg/kg,标准加入5～100μg/kg的平均回收率为95.40%～98.00%。该方法具有操作简便、可靠、灵敏度高、定量准确等优点,可用于焙烤食品中的氨基甲酸乙酯检测。

A method for the determination of ethyl carbamate in baking foods by matrix solid phase dispersion and gas chromatography tandem mass spectrometry has been developed.The samples were extracted by the matrix solid phase dispersion in the chromatography column after absorbing by diatomite,the samples were cleaned up nonpolar components with hexane and rinsed with dichloromethane,and the GC analysis was carried out by DB-225MS capillary column and GC/MS/MS.The developed method exhibited good linear over the range from 5 μg/L to 500 μg/L with a correlation coefficient of 0.9997,the limit of detection was 2.5 μg/kg.The average recoveries were 95.40% to 98.00% by stand addition method in 5 μg/kg to 100 μg/kg.This method was simple,reliable,sensitive and accurate.A useful method for determining ethyl carbamate in baking foods was provided for forensic analysis.