固相萃取-气相色谱-质谱法测定白酒中氨基甲酸乙酯  

Determination of ethyl carbamate in wine by solid phase extraction and gas chromatography-mass spectrometry

作　　者：单美娜[1] 徐晓枫[1] 蒲云霞[1] 陈志民[1] 李伟[1] 

机构地区：[1]内蒙古自治区疾病预防控制中心,内蒙古呼和浩特010030

出　　处：《中国卫生检验杂志》2014年第15期2149-2150,共2页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立酒中氨基甲酸乙酯的气相色谱-质谱测定方法。方法样品经硅藻土固相萃取柱净化,用10 ml 5%乙酸乙酯/乙醚洗脱,经过无水硫酸钠脱水,在30℃下用氮气缓缓吹至近干,用甲醇(色谱纯)定容至1.0 ml。以气相色谱-质谱选择44,62,89等3个碎片离子进行定性定量分析。结果氨基甲酸乙酯定量分析在20 ng/ml～160 ng/ml呈良好的线性关系,相关系数为0.9990,检出限2.0μg/kg,平均回收率为80.8%～91.3%,RSD为3.71%。结论该方法适合酒中氨基甲酸乙酯的检测。Objective To establish a method for the determination of ethyl carbamate in wine by gas chromatography-mass spectrometry. Methods The sample was purified by diatomite solid phase extraction,and eluted by 10 ml 5% ethyl acetate ether,and dehydrated by anhydrous sodium sulfate. Then the sample was slowly blowed to nearly dry with nitrogen at 30 ℃,and dissolved at 1. 0 ml by methanol（HPLC purity）. The fragment ions 44,62,89 were selected for qualitative and quantitative analysis by gas chromatography-mass spectrometry. Results Ethyl carbamate showed good linearity in the range of 20 ng/ml ～160 ng/ml with the relative coefficients of 0. 9990. The limit of detection was 2. 0 μg/kg. The average recoveries were between80. 8% ～ 91. 3% and the relative standard derivation was 3. 71%. Conclusion This established method can be applied to determine the ethyl carbamate in wine.

关 键 词：固相萃取 气相色谱-质谱法 氨基甲酸乙酯 

分 类 号：O657.63[理学—分析化学]