气相色谱-串联质谱法测定黄酒和酱油中的氨基甲酸乙酯
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 Extrelut TM NT 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 2 ?g/kg 和 5~1000 ?g/kg (R＞0.999)。在 50、200、500 ?g/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、200 ?g/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 car-bamate 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 Extre-lut TM NT column for matrix solid-phase dispersion extraction. Hexane was added to wash the matrix interfe-rences 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 levels of 50, 200, and 500 μg/kg were 97.4%~98.8% with the RSD of 4.0%~8.4% respectively. 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% respectively. Conclusion The method ishighly 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.
标题：气相色谱-串联质谱法测定黄酒和酱油中的氨基甲酸乙酯
英文标题：Determination of ethyl carbamate in Chinese rice wine and soy sauce by gas chromatography-tandem mass spectrometry
作者：
徐小民 浙江省疾病预防控制中心
何华丽 浙江工业大学化学工程与材料科学学院
阮瑜迪 浙江工业大学化学工程与材料科学学院
黄百芬 浙江省疾病预防控制中心
任一平 浙江省疾病预防控制中心
中文关键词:饮料氨基甲酸乙酯,黄酒,酱油,气相色谱串联质谱法,同位素内标法,
英文关键词:ethyl carbamate,Chinese rice wine,soy sauce,gas chromatography-tandem mass spectrometry,isotope labeled internal standard,
发表日期：2013-05-22
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