SPE-GC/MS外标法测定酒中氨基甲酸乙酯

Determination of Ethyl Carbamate in Wine by SPE-GC/MS with External Standard Method

建立固相萃取(SPE)结合气相色谱质谱联用仪(GC/MS)测定酒中氨基甲酸乙酯。试样经硅藻土固相萃取柱净化,乙酸乙酯/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外标法对其进行定性、定量。氨基甲酸乙酯在10—120μg/L浓度范围内线性关系良好,r2=0.9993,检测限为1.6μg/kg,定量限为3.0μg/kg,加标回收率在81.0%—97.4%之间,RSD为2.6%—5.5%(n=6)。应用此方法,对市场销售的各种酒进行了检测,氨基甲酸乙酯的含量在5.8—93.6μg/kg之间。此方法可靠、便捷,净化效果好,灵敏度、准确度均满足检测要求,可作为酒中氨基甲酸乙酯含量的检测方法。

The study established a method for determination of ethyl earbamate in wine by solid phase extraction （SPE） and gas chro- matograph-mass spectrometry （GC/MS） . The samples were extracted by the SPE little diatomite column, then washed with ethyl acetate/ ether elution. Determination and confirmation were performed by GC/MS at selective ionsmonitoringmode with external standard method. The calibration curve showed a good linear relationship in the range of 10--120μg,/L, and the correlation coefficient r2 was 0. 9993, The lowest concentration determined was 1.6μg/kg, and quantitative limits was 3.0μg/kg. The extraction recovery was 81.0%--97.4% , and the RSD was 2. 6% --5.5% （n = 6） . The method was sensitive, accurate and could be used for determination of ethyl carbamate in wine.