气相色谱-串联质谱法测定黄酒和酱油中的氨基甲酸乙酯

Determination of ethyl carbamate in Chinese rice wine and soy sauce by gas chromatography-tandem mass spectrometry

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 qualitative and quantitative determination of ethyl carbamate in Chinese rice wine and soy sauce by gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods After spiked with internal standard ethyl carbamate-d5,the sample was directly loaded to an ExtrelutTM NT column for matrix solid-phase dispersion extraction.Hexane was added to wash the matrix interferences and 90%(v/v) ethyl ether/ethyl acetate mixture was used to elute the analyte.The concentrated extract was detected by GC-MS/MS with multiple reaction monitoring(MRM) mode.Results The limit of detection(LOD) was 2 μg/kg and the linear range was 5~1000 μg/kg(R>0.999).For Chinese rice wine,the recoveries at the spiked levels of 50,200,and 500 μg/kg were 97.4%~98.8% with the RSD of 4.0%~8.4%.For soy sauce,the recoveries at the levels of 10,50,and 200 μg/kg were 96.2%~104.0% with the RSD of 5.3%~10.0%.Conclusion The method is highly sensitive,easy operating,accurate for quantitative analysis,and reliable for qualitative detection.It is suitable for determination of ethyl carbamate in Chinese rice wine and soy sauce.