酒中氨基甲酸乙酯的测定分析

Determination of Ethyl Carbamate in Wines

目的建立酒中氨基甲酸乙酯含量的测定方法。方法以氘代同位素为内标,采用硅藻土固相萃取柱进行萃取,乙醚洗脱,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2.0μg/L,回收率为91.0%-102.0%,RSD为1.8%。采用本方法测定了河南市场上13种葡萄酒、25种白酒、12种黄酒、5种调料酒中氨基甲酸乙酯含量,结果为：葡萄酒3.5-246.4μg/kg、白酒6.9-485.5μg/kg、黄酒10.4-332.9μg/kg、调料酒24.9-49.1μg/kg。结论本方法精密度和准确度高,且简便快捷,适用于酒中氨基甲酸乙酯的测定。

Objective To establish a method for determination of ethyl carbamate in wines. Methods The samples were isolated and concentrated by florisil solid - phase extraction cartridges, followed by elution with ether. With the deuterated isotopes as internal standard, the determination was carried out by gas chromatography - mass spectrometry with selected ion monitoring mode. Results The detection limit was 2. 0 μg/L. The recoveries of ethyl carbamate ranged from 91.0% to 102. 0% ,with the RSD of 1. 8%. The determination results of the wines in markets of Henan province showed that the concentrations for ethyl carbamate in 13 grape wines ,25 liquors, 12 yellow rice wines, and 5 cooking wines were in the range of 3.5 - 246. 4 μg/kg,6. 9 - 485.5μg/kg, 10.4 - 332. 9 μg/kg, and 24.9 - 49.μg/kg, respectively. Conclusion The proposed method is characterized by simplicity, high sensitivity and accuracy, it is suitable for the determination of ethyl carbamate in grape wines, yellow rice wines,liquors and cooking wines.