1 Key Laboratory of Industrial Fermentation Microbiology, Ministry of Education, Tianjin University of Science and Technology, Tianjin, 300457, People's Republic of China.
2 Tianjin Key Laboratory of Industrial Microbiology, College of Biotechnology, Tianjin University of Science and Technology, Tianjin, 300457, People's Republic of China.
J Food Prot. 2019 Aug;82(8):1377-1383. doi: 10.4315/0362-028X.JFP-18-594.
In this study, a novel method using gas chromatography-mass spectrometry coupled with ethanol and KHPO aqueous two-phase system (ATPS) was established for the quantitative determination of trace ethyl carbamate (EC) in red wine. The parameters that influence EC extraction in an aqueous two-phase system, including extraction temperature, time, pH, and ethanol concentration, were optimized. Method validation results indicated that the regression coefficient of the proposed method was 0.9979 in the linear range of 10 to 100 μg/L, and the limits of detection and quantification were 2.8 and 9.2 μg/L, respectively. Four red wine samples made from different grape varieties were processed by the proposed method for the repeatability verification, and EC concentrations were between 15.8 and 37.3 μg/L, with the relative standard deviations ranging from 3.5 to 6.6%. Results of the precision assay showed the average recovery of EC in red wine at 95.4 to 107.1%, with the relative standard deviations ranging from 1.4 to 6.2%. This method proved to be simple and reliable for quantitative determination of trace EC in red wine and would give guidance for quality monitoring of various red wines in the production process.
本研究建立了一种使用气相色谱-质谱联用技术结合乙醇和 KHPO4 双水相体系(ATPS)的新方法,用于定量测定红酒中的痕量氨基甲酸乙酯(EC)。优化了影响双水相体系中 EC 萃取的参数,包括萃取温度、时间、pH 值和乙醇浓度。方法验证结果表明,该方法在 10 至 100μg/L 的线性范围内回归系数为 0.9979,检测限和定量限分别为 2.8 和 9.2μg/L。采用所提出的方法对来自不同葡萄品种的 4 个红酒样品进行重复性验证,EC 浓度在 15.8 至 37.3μg/L 之间,相对标准偏差在 3.5 至 6.6%之间。精密度测定结果表明,EC 在红酒中的平均回收率为 95.4%至 107.1%,相对标准偏差在 1.4%至 6.2%之间。该方法简单可靠,可用于定量测定红酒中的痕量 EC,为生产过程中各种红酒的质量监测提供指导。