顶空-固相微萃取-气质联用技术快速测定黄酒中氨基甲酸乙酯的方法研究

Rapid determination of ethyl carbamate in Chinese rice wine by HS-SPME and GC-MS

黄酒中含有微量氨基甲酸乙酯(Ethyl Carbamate,EC),对人体健康有潜在不利影响,对其含量的准确测定是监管与控制的基础。采用顶空-固相微萃取-气质联用技术(HS-SPME-GC-MS),建立了完全自动化、快速简便测定黄酒中EC的方法。结果表明,以氨基甲酸丙酯为内标,优化的参数为:添加NaCl至0.39g/mL酒样,采用聚丙烯酸酯(PA)萃取头70℃下萃取45min。此方法线性相关系数R为0.9983,回收率为90.21%～99.07%,相对标准偏差小于2.5%,检测限低至1.19μg/L。此EC快速测定方法无需繁琐的预处理过程,自动快速高效,连续分析中单个样品平均总需时只要50min,且无有机溶剂危害,推荐作为黄酒中EC含量测定的标准方法之一。

Ethyl carbamate（EC）is known to be harmful to human health and usually found in Chinese rice wine.The supervision and control of EC premise on the accurate determination.A fully automated procedure using headspace solid-phase microextraction（HS-SPME）followed by gas chromatographic-mass specometric（GC-MS）detection was developed for quick determination of EC in Chinese rice wine.Using propyl carbamate（n-PC）as internal standard,the optimised HS-SPME extraction was 45min at 70℃ with Polyacrylic（PA）fibre after the addition of NaCl to 0.39g/mL.This method exhibited good linearity with a regression coefficient of 0.9983.The recovery,relative standard deviation,and limits of detection were 90.21% ～ 99.07%,lower than 2.5%,and 1.19μg/L,respectively.The HS-SPME-GC-MS procedure requiring little operator effort was suitable for the automated,rapid,convenient,and inexpensive determination of EC in Chinese rice wine.One sample only took altogether 50min in continuous detection.And this solvent-free procedure was recommended as one of the standard procedures for the determination of EC in Chinese rice wine.