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目的建立分散液液萃取-气相色谱质谱测定酒精饮料中氨基甲酸乙酯的方法。方法取5 ml酒样,加入氯化钠振荡溶解后,以5 ml乙醚(含内标50 ng/ml)作为萃取剂注入样液,利用酒样中含有的乙醇作为分散剂进行乳化分散,离心后取上层有机相氮吹至干,用0.5 ml甲醇溶解残渣后进样分析。气相色谱采用DB-WAX毛细色谱柱程序升温分离,选择离子监测模式检测,内标法定量。结果氨基甲酸乙酯在1.0~100 ng/ml范围内线性良好,方法检出限为0.11ng/ml,精密度为2.33%~6.92%,加标回收率为77.8%~101%。结论所建立方法具有简单、灵敏准确的特点,适用于酒精饮料中氨基甲酸乙酯的测定。
Objective To establish a method for the determination of urethane in alcoholic beverage by dispersive liquid-liquid chromatography-gas chromatography-mass spectrometry. Methods Take 5 ml wine sample, dissolve it in sodium chloride, dissolve in 5 ml diethyl ether (containing 50 ng / ml internal standard) as extractant, inject the sample solution with ethanol as dispersant and centrifuge After taking the upper organic nitrogen blowing to dry, with 0.5 ml of methanol dissolved residue after injection analysis. Gas chromatography using DB-WAX capillary column temperature program, selected ion monitoring mode detection, internal standard method. The results showed that the linear range was 1.0-100 ng / ml. The detection limits were 0.11ng / ml, the precision was 2.33% ~ 6.92%, and the recoveries were 77.8% ~ 101%. Conclusion The established method is simple, sensitive and accurate. It is suitable for the determination of urethane in alcoholic beverages.