Determination of Ethyl Carbamate in Sake Using Headspace Solid Phase Microextraction

Abstract

An analytical method for the determination of ethyl carbamate in alcoholic beverages has been developed and optimized. A combination of headspace solid phase microextraction (HS-SPME), as the extraction technique, and GC/MS, as the determination technique, was utilized. Analytical grade ethyl carbamate dissolved in ethanol solution was analyzed to determine the optimum analytical conditions. Ethyl carbamate-d5 was added as an internal standard. The following HS-SPME conditions were investigated: type of stationary phase of the fibre, ethanol content, sample volume and extraction time. The optimized procedure showed that the detection limit, relative standard deviation, and recovery were 6.7 μg/L, 0.4–2.0%, and 103.6–107.6%, respectively. The precision of this new method was equivalent to previous analyses. Finally, the developed method was applied to the analysis of ethyl carbamate in sake.