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目的建立气相色谱-串联质谱法(GC-MS/MS)测定黄酒和酱油中氨基甲酸乙酯的分析方法。方法样品添加同位素内标氨基甲酸乙酯-d5后,直接上样到填装好ExtrelutTMNT有机硅藻土的柱中进行基质固相分散萃取,先用正己烷淋洗除杂,再用乙酸乙酯:乙醚(1:9,v/v)的混合溶剂洗脱氨基甲酸乙酯,洗脱液经浓缩后采用GC-MS/MS多反应监测(MRM)模式测定。结果方法检出限和线性范围分别为2μg/kg和5～1000μg/kg(R>0.999)。在50、200、500μg/kg三个添加水平下,黄酒基体中氨基甲酸乙酯的加标回收率为97.4%～98.8%,RSD为4.0%～8.4%。向酱油基体中添加10、50、200μg/kg三个浓度水平,氨基甲酸乙酯的加标回收率为96.2%～104.0%,RSD为5.3%～10.0%。结论该方法定量准确、操作简单、灵敏度高、定性确证可靠,适用于黄酒和酱油中氨基甲酸乙酯的测定。
Objective To establish a method for the determination of urethane in rice wine and soy sauce by gas chromatography-tandem mass spectrometry (GC-MS / MS). Method The sample was added with isotopic internal standard urethane-d5 and directly loaded onto a column filled with Extrelut TNM organic diatomaceous earth for matrix solid-phase dispersion extraction. The sample was first rinsed with n-hexane to remove impurities and then extracted with ethyl acetate : Ethyl carbamate was eluted with a mixed solvent of diethyl ether (1: 9, v / v). The eluent was concentrated and determined by GC-MS / MS multiple reaction monitoring (MRM). Results The detection limit and linear range were 2μg / kg and 5 ~ 1000μg / kg respectively (R> 0.999). The spiked recoveries of urethane in the rice wine matrix were 97.4% ~ 98.8% and the RSD was 4.0% ~ 8.4% at the three levels of 50, 200 and 500 μg / kg. The concentration of 10, 50, 200μg / kg was added to the soy sauce matrix. The spiked recoveries of urethane were 96.2% -104.0% with RSD of 5.3% -10.0%. Conclusion The method is accurate, simple, sensitive and reliable. The method is suitable for the determination of urethane in rice wine and soy sauce.