建立了高效液相色谱-荧光法检测酱油中氨基甲酸乙酯的分析方法.首先用乙酸乙酯萃取酱油中的氨基甲酸乙酯,再经减压旋转蒸发浓缩得待测样品.其次确定了衍生化反应条件:取1.0 mL待测样品,加入200 μL 0.02 mol/L占吨醇,再加入100 μL 1.5 mol/L盐酸于暗处反应30min.实验结果表明:该方法标准曲线良好,线性范围为10～200 μg/L,相关系数为R2=0.988,氨基甲酸乙酯的出峰时间为14.882 min,平均回收率为100.12％.最低检测限为5μg/L,比已经发表的最低检测限(20 μg/L)要低.最后对市售酱油S1～S6样品中的氨基甲酸乙酯含量进行了检测,表明市售酱油S1～S6中氨基甲酸乙酯的含量为31.25～114.78μg/L.本文所建立的方法具有简便快捷、灵敏度高的特点,可满足对酱油中氨基甲酸乙酯含量检测的需要.%A high performance liquid chromatography with fluorescence detection method was established for the determination of ethyl carbamate (EC) in soy sauce. First, the ethyl carbamate was extracted with ethyl acetate. Then, the supernatant was concentrated by vacuum-rotary evaporation. The resulting samples were applied to fluorescence derivatization. The reaction conditions were as follows: 1.0 mL sample, 200 μL 0.02 mol/L xanthydrol and 100 μL 1.5 mol/L HC1 were added into 5 mL test tubes and incubated in the dark for 30 min. The linear range of this method was 10 to 200 μg/L and the correlation coefficient between EC concentration and the fluorescence response of HPLC were 0.988. The detectable limit was 5 μg/L, significantly better than the previous best reported detection limit of 20 μg/L. Six samples of soy sauce purchased from supermarket were assayed with this method. It was demonstrated that it was a simple and convenient assay method for quantifying EC concentration in soy sauce.
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