气相色谱质谱法同时测定黄酒中氨基甲酸甲酯和氨基甲酸乙酯  

Detection of methyl carbamate and ethyl carbamate in yellow rice wine by gas chromatography-mass spectrometry

作　　者：吴平谷[1] 马冰洁[1] 王立媛[1] 沈向红[1] 张晶[1] 谭莹[1] 姜维[1] 

机构地区：[1]浙江省疾病预防控制中心食品检验科,杭州310051

出　　处：《中华预防医学杂志》2013年第11期1056-1059,共4页Chinese Journal of Preventive Medicine

摘　　要：目的 建立黄酒中氨基甲酸甲酯（MC）和氨基甲酸乙酯（EC）同时测定的气相色谱质谱方法.方法 黄酒中MC和EC经9-占吨醇衍生后,用气相色谱质谱法（GC/MS）测定两种衍生物,采用D5-EC同位素内标法进行定量分析.结果 本测定方法MC和EC的线性范围为2.0～ 400.0 μg/L,相关系数分别为0.998和0.999,定量限和检出限分别为0.67和2.0μg/kg,黄酒中加入2.0 ～ 300.0 μg/kg MC和EC,日内平均回收率为78.8％ ～102.3％,相对标准偏差为3.2％～11.6％,日间平均回收率为75.4％ ～ 101.3％,相对标准偏差为3.8％ ～13.4％.采用本方法对市场上20份黄酒中MC和EC进行检测,MC含量为未检出～1.2 μg/kg,检出率为6％（3/20）,EC含量范围为18.6～432.3 μg/kg,平均含量为135.2 μg/kg.结论 本方法具有操作简便、快速等优点,适用于黄酒中MC和EC的同时检测.Objective To establish the method of simultaneous determination of methylcarbamate （MC） and ethylcarbamate （EC） in yellow rice wine by gas chromatography-mass spectrometry （GC/MS）.Methods MC and EC in yellow rice wine were derived by 9-xanthydrol,and then the derivants were detected by GC/MS; and quantitatively analyzed by DS-EC isotope internal standard method.Results The linearity of MC and EC ranged from 2.0 μg/L to 400.0 μg/L,with correlation coefficients at 0.998 and 0.999,respectively.The limits of quantitation （LOQ） and detection （LOD） were 0.67 and 2.0 μg/kg.When MC and EC were added in yellow rice wine at the range of 2.0-300.0 μg/kg,the intraday average recovery rate was 78.8％-102.3％,relative standard deviation was 3.2％-11.6％ ; interday average recovery rate was 75.4％-101.3％,relative standard deviation was 3.8％-13.4％.20 samples of yellow rice wine from supermarket were detected using this method,the contents of MC were in the range of ND （no detected） to 1.2 μg/kg,the detection rate was 6％ （3/20）,the contents of EC in the range of 18.6 μg/kgto 432.3 μg/kg,with the average level at 135.2 μg/kg.Conclusion The method is simple,rapid and useful for simultaneous determination of MC and EC in yellow rice wine.

关 键 词：气相色谱-质谱法 酯类 酒精性饮料 

分 类 号：TS261.7[轻工技术与工程—发酵工程] O657.63[轻工技术与工程—食品科学与工程]