SPME结合气质联用测定不同发酵阶段黄酒中氨基甲酸乙酯的研究.doc

SPME结合气质联用测定不同发酵阶段黄酒中氨基甲酸乙酯的研究 摘 要：氨基甲酸乙酯（EC）已被证明是一种致癌物质。本实验获取黄酒中的氨基甲酸乙酯的方法为固相微萃取（SPME），然后结合色谱检测氨基甲酸乙酯的含量。实验结果表明：固相微萃取所使用的萃取头型号为50/30μmDVB/CAR/PDMS，获取氨基甲酸乙酯的最佳条件为：每100mL酒样中加入1.5mL浓度为300g/L的氢氧化钠溶液调节pH 值后取5mL样液，加入固体氯化钠的量为1.0g，原酒样的酒精度17.4度，最佳稀释度为20%，样品处理温度为70℃，预处理时间为20min。此时可以得到较好的氨基甲酸乙酯的色谱图，线性方程为y=82.445x-102.68，其线性相关系数为0.9969。本方法的回收率为103.16%～107.01%etermination of ethyl carbamate (EC) in rice wines of different fermenting stages by SPME combined with GC-MS Abstract：Ethyl carbamate?(EC)?has been?proved to be a?carcinogen. In this study,?rice wine?for?ethyl carbamate?in?solid phase micro-extraction?method?(SPME), then combined with?chromatography?the content of?ethyl carbamate. The results show that：SPME?extraction?of the?first?model?to use 50/30μmDVB/CAR/PDMS, Solid?urethane?to obtain?the best conditions are: 100mL?wine samples?for each?concentration of?added 1.5mL 300g/L sodium hydroxide solution?pH?value?adjusted?to take 5mL sample solution, The amount?of solid?sodium chloride?is added?1.0g, Kind of?alcoholic?liquor?of 17.4 degrees, the best?20%? dilution,?the sample?treatment temperature?is 70 ℃,?pretreatment?time was 20min.?At this point?you can?get a better?chromatograms?of ethyl carbamate, the linear equation y = 82.445x-102.68,??the linear correlation coefficient of?0.9969.??The recoveries of? the method ranges from?103.16% to 107.01%. Different fermentation?time?to take?1 day?to 13 days of?wine samples, measured by the?ascending order of?ethyl?carbamate;??take a different?wine?wine samples?in early?years?to 5?years?old wine to?sample,?the measured EC Levels also were increased.?In this study,?the?clear results?obtained?for?rice wine production and?quality control?in?the data?description. Key words: EC， SPME GC-MS， rice wine 1.前言 1 1.1本课题的国内外研究现状 1 1.1.1氨基甲酸乙酯毒性概述 1 1.1.2 氨基甲酸乙酯的形成机理 1 1.1.3 氨基甲酸乙酯物化性质 2 1.1.4 氨基甲酸乙酯监测标准及背景 2 1.1.5 氨基甲酸乙酯的获取方法 3 1.1.6氨基甲酸乙酯的检测方法 5 1.2 本课题的研究目的和意义 7 2材料与方法 8 2.1 实验材料及仪器 8 2.1.1 实验材料及试剂 8 2.1.2 主要设备和仪器 8 2.2 氨基甲酸乙酯标准溶液的制备 9 2.2