分散液液萃取-气相色谱/质谱法测定酒精饮料中氨基甲酸乙酯  

Determination of ethyl carbamate in alcoholic beverage Dispersive liquidliquid extraction combined with gas chromatography-mass spectrometry

作　　者：袁悦[1] 王倩[1] 王佳敏[1] 黄欢[1] 张丽[1] 邹晓莉[1] 

机构地区：[1]四川大学华西公共卫生学院(华西第四医院),四川成都610041

出　　处：《现代预防医学》2017年第14期2618-2622,共5页Modern Preventive Medicine

基　　金：四川大学省级创新创业项目

摘　　要：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 The objectiveof the study was todevelop a method for the determination ofethyl carbamate in alcoholic beverage Dispersive liquid-liquid extraction combined with gas chromatography-mass spectrometry（DLLE-GC/MS）. Methods Sodium chloride was added into 5mL of alcohol beverages sample to increase ionic strength. 5mL diethyl ether （containing 50 ng/mL internal standard） as extraetant was injected into sample solution and mixed with ethanol as dispersant to make it emulsified and dispersed. After the mixed solution being centrifuged, organic phase was collected and concentrated via nitrogen flow. The residue was resolved and diluted by 0.5mL methanol for GC/MS analysis. Chromatographic separation was achieved by DB-WAX with temperature programming. Selected ion monitoring （SIM） mode was used in mass spectrometric analysis and quantitative analysis was completed by internal standard method. Results Ethyl carbamateexhibited a good linear relationship at 1.0-100ng/mL, detection limit of the method was 0.11ng/mL, the relative standard deviation （RSD） was 2.33% -6.92%, and the average recovery rate of thesamples ranged between77.8% and 101%. Conclusion The method is simple, accurate, and high in sensitive, and can be used for the determination of ethyl carbamate in alcohol beverages.

关 键 词：气相色谱-质谱法 酒精饮料 氨基甲酸乙酯 分散液液萃取 

分 类 号：R155.5[医药卫生—营养与食品卫生学]