白酒中氨基甲酸乙酯检测方法比较

建立并使用了高效液相色谱法(HPLC)与气相色谱-质谱联用法(GC-MS)两种白酒样品中EC的检测方法,两种方法定量分析的线性关系良好,相关系数在0.997以上。其中HPLC法检出限为4.0μg/L,回收率在84.9%~105.1%之间,RSD<6.84%;GC-MS法检出限为1.3μg/L,GC-MS检测回收率在95.3%~104.7%之间,RSD<4.26%。结果显示,两种方法的准确性和重复性均符合实验要求。其中HPLC法具有前处理操作方便,且试剂毒性相对较低的优点,但GC-MS方法的精确性和稳定性则比HPLC法更高,且检出限更低、总体处理及进样时间更短,单位时间内能更快、更精确地对酒样中氨基甲酸乙酯进行检测。结合产业实际发展情况,白酒的氨基甲酸乙酯检测量日益增多,检测限要求更低,故使用GC-MS法检测白酒中的氨基甲酸乙酯更能满足今后的检测工作需求。

Comparison of Two Detection Methods of Ethyl Carbamate in Baijiu

Two detection methods of EC in Baijiu including HPLC and GC-MS were compared.Both methods had good linear relationship of quantitative analysis with the correlation coefficients above 0.997.The detection limit of HPLC was 4.0μg/L,its recovery rate was between 84.9%to 105.1%,and RSD was less than 6.84%.The detection limit of GC-MS was 1.3μg/L,its recovery rate was between 95.3%to 104.7%,and RSD was less than 4.26%.The accuracy and repeatability of both methods could meet the requirements.HPLC had simpler pretreatment and its reagents had much lower toxicity.However,the accuracy and the stability of GCMS were better than HPLC,its detection limit was lower,its sampling time was shorter,and EC detection was faster.In consideration of the practical situations such as increasing EC detection tasks and the requirements of low detection limit etc.,GC-MS is recommended for the detection of EC in Baijiu in practice.