气相色谱-质谱法测定白酒中氨基甲酸乙酯的分析

Determination of Methyl Carbamate and Ethyl Carbamate in White Liquor by GC-MS

探讨气相色谱-质谱法测定白酒中氨基甲酸乙酯的分析方法。白酒中氨基甲酸乙酯经过硅藻土固相萃取柱净化富集，再将洗脱液浓缩定容，用气相色谱-质谱仪测定，通过目标组分的质谱图和保留时间与目标组分的标准将物质的质谱图和保留时间对照进行定性，内标法定量。样品加标回收率为87％～110％，相对标准偏差为0．95％～2．35％，检出限为0．23ng／mL。结果表明，利用DB—INNOWAX型毛细管色谱柱分离目标物效果好，采用硅藻土萃取柱富集净化氨基甲酸乙酯回收率高，完全可以满足白酒中氨基甲酸乙酯的测定。

Gas chromatography/mass spectrometry method for the determination of ethyl carbamate in liquor is discussed, to study ethyl carbamate in hquor by diatomite solid phase extraction column enrichment and purification, the eluent concentration constant volume, with gas chromatography-mass spectrometry determination of the target analytes, the mass spectrum and the retention time and the target analytes standard material mass spectrum and the retention times of light qualitative, internal standard method quantitative. The rate of recovery is 87%-110%, and relative standard deviation of 0.95%-2.35%, the detection limit is 0.23 ng/mL. The experimental results show that using DB-INNOWAX capillary chromatographic column for the separation of the target effect is good, the use of diatomite in extraction column and purifying ethyl carbamate recovery rate is high, can fully meet the determination of ethyl carbamate in liquor.