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目的:建立一种快速、准确测定黄酒中氨基甲酸乙酯(EC)含量的气相色谱-质谱(GC/MS)法。方法:酒样添加d5-EC同位素内标,经硅藻土层析柱吸附,乙醚洗脱,用GC/MS测定,内标法定量。色谱柱为HP-INNOWAX石英毛细管柱(30 m×0.25 mm×0.25μm)。结果:进行高、中、低三个浓度水平的加标回收试验,平均回收率为89.2%～102%,RSD为2.2%～4.7%(n=6)。应用本方法检测了55份广东本地生产的黄酒产品,检出率为100%,含量范围10μg/kg～1200μg/kg。结论:该方法快速、准确、分析成本低,能满足大批量酒类样品中氨基甲酸乙酯快速分析的要求。
Objective: To establish a rapid and accurate gas chromatography - mass spectrometry (GC / MS) method for the determination of urethane (EC) in rice wine. Methods: The d5-EC isotope internal standard was added into wine samples, adsorbed on celite column and eluted with diethyl ether. The internal standard was determined by GC / MS and internal standard method. The column was a HP-INNOWAX quartz capillary column (30 m × 0.25 mm × 0.25 μm). Results: The average recoveries were 89.2% ~ 102% with RSD of 2.2% ~ 4.7% (n = 6). Using this method, 55 samples of yellow rice wine produced locally in Guangdong were detected. The detection rate was 100% and the content range was 10μg / kg ~ 1200μg / kg. Conclusion: The method is rapid, accurate and low in cost. It can meet the requirement of rapid urethane analysis in large quantities of alcoholic samples.