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目的建立液-液萃取稳定同位素稀释测定酒中氨基甲酸乙酯含量的方法。方法以氘代同位素D5-氨基甲酸乙酯为内标,用液-液萃取法稳定同位素稀释,气相色谱-质谱选择离子法测定。结果氨基甲酸乙酯的检出限为1.1μg/kg,回收率为90.7%~106.3%,RSD为2.6%。测定市售10种葡萄酒、15种白酒和20种黄酒,氨基甲酸乙酯含量分别为:葡萄酒5.57~20.7μg/kg、白酒5.8~297μg/kg、黄酒79.8~498μg/kg。结论液-液萃取法精密度和准确度高,简便快速,适用于酒中氨基甲酸乙酯的测定。
Objective To establish a method for the determination of urethane in wine by liquid-liquid extraction and stable isotope dilution. Methods Deuterated isotope D5-urethane was used as internal standard and was subjected to stable isotope dilution by liquid-liquid extraction and determined by gas chromatography-mass spectrometry. Results The detection limit of urethane was 1.1μg / kg, the recovery was 90.7% -106.3% and the RSD was 2.6%. Determination of commercially available 10 kinds of wine, 15 kinds of white wine and 20 kinds of rice wine, ethyl carbamate content were: wine 5.57 ~ 20.7μg / kg, liquor 5.8 ~ 297μg / kg, rice wine 79.8 ~ 498μg / kg. Conclusion The liquid-liquid extraction method has high precision and accuracy, is simple and rapid, and is suitable for the determination of urethane in wine.