Research Center of Analysis and Measurement, Fudan University, Shanghai, China.
J Sep Sci. 2012 Apr;35(7):804-10. doi: 10.1002/jssc.201100526. Epub 2012 Mar 2.
A sensitive and rapid analytical methodology based on derivatization followed by gas chromatography-mass spectrometry (GC-MS) was developed for the quantitative determination of the toxic contaminant ethyl carbamate (EC, urethane, C(2)H(5)OCONH(2)) in alcoholic samples. EC was extracted using liquid-liquid extraction technique, and then silylated with bis-(trimethylsilyl)trifluoroacetamide, analysed finally by GC-MS. The isopropyl carbamate was used as the internal standard for quantitative analysis of EC in alcoholic samples. In this work, the sample extraction and derivatization reaction conditions were investigated, and the optimal extraction conditions obtained were: pH 9 and solvent of ethyl acetate, and the derivatization conditions were: derivatization reaction temperature of 80°C and time duration of 30 min. With the optimal conditions, the method validations were also studied. In the validation studies, EC exhibited good linearity with a regression coefficient of 0.9999. The limit of detection and limit of quantification were 0.30 and 5.0 μg/kg, respectively. The precision was less than 8.4%. Finally, the proposed technique was successfully applied to the analysis of EC in 35 kinds of alcoholic samples. The experimental results have demonstrated that the proposed technique is a fast, reliable and low-cost method for determination of EC in alcoholic samples.
建立了一种基于衍生化后气相色谱-质谱联用(GC-MS)的灵敏、快速分析方法,用于定量测定酒精样品中的有毒污染物氨基甲酸乙酯(EC,尿烷,C(2)H(5)OCONH(2))。采用液液萃取技术提取 EC,然后用双(三甲基硅基)三氟乙酰胺硅烷化,最后用 GC-MS 分析。异丙基氨基甲酸酯被用作酒精样品中 EC 定量分析的内标。在这项工作中,研究了样品提取和衍生化反应条件,并获得了最佳的提取条件:pH 9 和乙酸乙酯溶剂,最佳的衍生化条件为:衍生化反应温度 80°C 和 30 分钟的时间持续时间。在最佳条件下,还研究了方法验证。在验证研究中,EC 表现出良好的线性关系,回归系数为 0.9999。检测限和定量限分别为 0.30 和 5.0 μg/kg,精密度小于 8.4%。最后,该技术成功应用于 35 种酒精样品中 EC 的分析。实验结果表明,该技术是一种快速、可靠、低成本的测定酒精样品中 EC 的方法。