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目的研究GC-MS法检测红葡萄酒中氨基甲酸乙酯的前处理方法和分析方法。方法比较2种不同的前处理方法,最后选用活性炭净化色素后,固相柱萃取,GC-MS法检测红葡萄酒中氨基甲酸乙酯。结果在前处理过程中,比较了2种不同前处理方法:(1)活性炭净化色素后,固相柱萃取方法回收率:低、中、高浓度回收率范围为70.9%～101.9%,平均87.1%;(2)固相柱萃取方法回收率:低、中、高浓度回收率范围为69.7%～96.1%,平均82.9%。所以选用活性炭净化色素-固相萃取法作为前处理方法,GC-MS法检测红葡萄酒中氨基甲酸乙酯,方法检出限20μg/ml,定量限10μg/kg,精密度2.0%,回收率87.1%,标准曲线相关系数r=0.9991。结论前处理方法提取净化效果显著,色谱柱柱温优化科学,能有效地分离检测红葡萄酒中氨基甲酸乙酯。
Objective To study the pretreatment method and analytical method of GC-MS for the determination of urethane in red wine. Methods Two different pretreatment methods were compared. Finally, activated carbon was used to purify the pigment, then the solid phase extraction and GC-MS were used to determine the ethyl carbamate in red wine. Results In the pretreatment, two different pretreatment methods were compared: (1) After the activated carbon purification pigment, the solid phase column extraction method recovery: low, medium and high concentration recovery range of 70.9% ~ 101.9%, an average of 87.1 %; (2) solid phase column extraction recovery: low, medium and high concentration recovery ranged from 69.7% to 96.1%, an average of 82.9%. Therefore, activated carbon purification pigment - solid phase extraction method as a pretreatment method, GC-MS detection of red wine, urethane detection limit of 20μg / ml, the limit of quantification 10μg / kg, precision 2.0%, recovery 87.1 %, The standard curve correlation coefficient r = 0.9991. Conclusion The pretreatment method has obvious purification effect and column temperature optimization science, which can effectively separate and detect the ethyl carbamate in red wine.