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.

abstractsObjective 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.