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目的建立顶空固相微萃取(HS-SPME)结合GC/MS分析酒精饮料中有毒污染物氨基甲酸乙酯(EC)的检测方法。方法试样中加入氘代同位素内标,萃取头采用70μm CW/DVB,2gNaCl,样品溶液pH7.0,70℃下萃取30min后,在气相色谱质谱仪进样口解析10min,DB-WAX毛细管柱气相色谱分离,选择离子监测(SIM)的质谱扫描模式进行定量分析。结果方法的线性范围在10～1000μg/L,检测限(S/N≥3)为1μg/L,定量限为10μg/L;不同基底样品中高低添加浓度的加标回收率为88.6%～94.7%,相对标准偏差值(RSD)为1.9%～3.6%。结论方法可靠、便捷且不需萃取溶剂,可全自动分析酒精饮料中氨基甲酸乙酯的含量。
Objective To develop a method for the determination of urethane (EC), a toxic pollutant in alcoholic beverages, by headspace solid-phase microextraction (HS-SPME) and GC / MS. Methods The deuterated isotope internal standard was added into the sample. The extraction head was extracted with 70μm CW / DVB, 2g NaCl, the sample solution was pH7.0 and extracted at 70 ℃ for 30min. The sample was analyzed by GC-MS for 10min. Gas chromatographic separation, selective ion monitoring (SIM) mass spectrometry scan mode for quantitative analysis. Results The linear range of the method was 10 ~ 1000μg / L, the limit of detection (S / N≥3) was 1μg / L, and the limit of quantification was 10μg / L. The recoveries of spiked samples from different basal samples were 88.6% ~ 94.7 %, And the relative standard deviation (RSD) was 1.9% ~ 3.6%. Conclusion The method is reliable, convenient and does not require solvent extraction. It can fully analyze the content of ethyl carbamate in alcoholic beverages.