GC-MS法测定酒中的氨基甲酸乙酯

Determination of ethyl carbamate in liquor by gas chromatography-mass spectrometry

目的：建立GC-MS法测定酒中氨基甲酸乙酯含量的方法,并利用该方法测定了不同种类酒中氨基甲酸乙酯的含量。方法：试样经硅藻土固相萃取柱净化,乙醚洗脱后,气相色谱-质谱联用仪测定,利用选择离子监测模式及内标法对其定性定量。结果：氨基甲酸乙酯在10～160μg/L浓度范围内线性关系良好,r=0.9994,最低检出浓度为4μg/L,回收率为93.3%～111.8%,RSD为3.4%～8.0%（n=5）,并且采用本方法测定了市售的10种黄酒、10种白酒、10种葡萄酒中氨基甲酸乙酯的含量,黄酒为6.0～80.6μg/kg,白酒为6.4～107.7μg/kg,葡萄酒为10.7～32.9μg/kg。结论：该方法准确可靠,可用于酒中氨基甲酸乙酯的含量测定。

Objective ：To develop a method for determination of ethyl carbamate （EC） in liquor by gas chromatography - mass spectrometry using deuterated isotope internal standard. Methods： The samples were extracted by the solid- phase extraction （SPE） little diatomite column, then washed with aethers. Determination and confirmation were performed by gas chromatography - mass spectrometry at selective ions monitoring mode with internal standard method. Results：The calibration curve was linear within the range of 10 - 160 μg/L,and the correlation coefficient r was 0. 9994. The lowest concentration determined was 4 μg/L. The extraction recovery was 93.3 % - 111.8 %, the RSD was 3.4% - 8.0% （ n = 5 ）. Conclusion： The method is accurate and suitable for the analysis of ethyl carbamate in liquor.