Pierce W M, Clark A O, Hurst H E
University of Louisville School of Medicine, Department of Pharmacology and Toxicology, KY 40292-0001.
J Assoc Off Anal Chem. 1988 Jul-Aug;71(4):781-4.
Quantitative methods are detailed for determination of ethyl carbamate in distilled alcoholic beverages by capillary gas chromatography with flame ionization detection (GC/FID) and by packed-column gas chromatography/mass spectrometry (GC/MS) using selected ion monitoring. Five g samples of distillate of known ethanol concentration are diluted with water to 25% ethanol (v/v), washed with petroleum ether, and extracted with dichloromethane prior to GC/FID or GC/MS analysis. As necessary, sample extracts that exhibit GC/FID interference are passed through alumina for additional cleanup. When internal standards (tert-butyl carbamate and n-butyl carbamate for GC/FID, or ethyl 13C-15N-carbamate for GC/MS) were used for quantitation, the limit of detection for ethyl carbamate was in the range of 5-25 ppb. Coefficients of variation ranged from 3.5 to 6.0% for GC/FID determinations, and from 1.4 to 3.2% for GC/MS. Correlation between methods for 22 random distillate samples ranging in concentration from approximately 40 to 800 ppb gave a correlation coefficient (r) of 0.996.
详细介绍了采用带有火焰离子化检测的毛细管气相色谱法（GC/FID）以及使用选择离子监测的填充柱气相色谱/质谱联用法（GC/MS）测定蒸馏酒精饮料中氨基甲酸乙酯的定量方法。将已知乙醇浓度的5g馏出物样品用水稀释至乙醇含量为25%（v/v），用石油醚洗涤，然后在进行GC/FID或GC/MS分析之前用二氯甲烷萃取。如有必要，对显示出GC/FID干扰的样品提取物通过氧化铝进行进一步净化。当使用内标（用于GC/FID的氨基甲酸叔丁酯和氨基甲酸正丁酯，或用于GC/MS的13C-15N-氨基甲酸乙酯）进行定量时，氨基甲酸乙酯的检测限在5-25 ppb范围内。GC/FID测定的变异系数范围为3.5%至6.0%，GC/MS测定的变异系数范围为1.4%至3.2%。对22个浓度范围约为40至800 ppb的随机馏出物样品进行的方法间相关性分析得出相关系数（r）为0.996。
