GC-MS法测定黄酒和食用酒精中的氨基甲酸乙酯  

Determination of ethylcarbamate in rice wine and edible alcohol by gas chromatography-mass spectrometry

作　　者：华颖 茅佩卿 刘柱 HUA Ying;MAO Peiqing;LIU Zhu(College of Pharmaceutical Sciences,Zhejiang Chinese Medical University,Hangzhou 310053,China;Zhejiang Institute for Food and Drug Control,Hangzhou 310052,China)

机构地区：[1]浙江中医药大学药学院,浙江杭州310053 [2]浙江省食品药品检验研究院,浙江杭州310052

出　　处：《食品与发酵工业》2019年第14期196-202,共7页Food and Fermentation Industries

基　　金：浙江省分析测试科技计划项目(2018C37044);浙江省基础公益研究计划项目(LGF18C200001)

摘　　要：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10~600μg/L线性关系良好,相关系数r^2=0.999 3。加标水平为5、100、250μg/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1.0μg/kg,方法的定量限为3.0μg/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 10-600μg/L with the correlation coefficient(r^2)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 1.0μg/kg and the quantitative limit was 3.0μg/kg.This method was accurate,sensitive and easy to operate,therefore,it is suitable for determining EC in rice wine and edible alcohol.

关 键 词：黄酒 食用酒精 氨基甲酸乙酯(ethylcarbamate EC) 气相色谱-质谱联用法(gas chromatography-mass spectrometry GC-MS) 

分 类 号：O657.63[理学—分析化学] TS261.7[理学—化学]