建立应用气相色谱-质谱联用法(gas chromatography-mass spectrometry, GC-MS)快速测定黄酒和食用酒精中氨基甲酸乙酯(ethylcarbamate, EC)的分析方法。以黄酒和食用酒精为研究对象,样品经过碱性硅藻土固相萃取柱净化、浓缩后,用GC-MS进行测定,同位素内标法定量。氨基甲酸乙酯在10~600 μg/L线性关系良好,相关系数r2=0.999 3。加标水平为5、100、250 μg/kg 3个浓度条件下,在黄酒中的加标回收率为81.2%~89.5%,每个加标水平测定6次的相对标准偏差(RSD)为3.7%~5.0%;在食用酒精中的加标回收率为91.2%~99.4%,每个加标水平测定6次的RSD为3.1%~4.1%。方法的检出限为1.0 μg/kg,方法的定量限为3.0 μg/kg。该方法定量准确、操作简便、灵敏度高,适用于黄酒和食用酒精中氨基甲酸乙酯的测定。
A rapid method for quantitative determination of ethylcarbamate (EC) in rice wine and edible alcohol was established by gas chromatography-mass spectrometry (GC-MS). Rice wine and edible alcohol were purified and concentrated by alkaline diatomaceous earth solid phase extraction column and then quantitatively determined by GC-MS with isotope internal standards. The linear range was 10-600 μg/L with the correlation coefficient (r2) of 0.999 3. The recovery rates were 81.2%-89.5% and 91.2%-99.4% for rice wine and edible alcohol, respectively, with the relative standard deviations (RSDs) were 3.7%-5.0% and 3.1%-4.1%, respectively. Furthermore, the detection limit was 1.0 μg/kg and the quantitative limit was 3.0 μg/kg. This method was accurate, sensitive and easy to operate, therefore, it is suitable for determining EC in rice wine and edible alcohol.
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