固相萃取-气相色谱-质谱法测定腐乳中氨基甲酸乙酯

Detection of ethyl carbamate in fermented bean curd by solid phase extraction-gas chromatography- mass spectrometry

中文关键词:  氨基甲酸乙酯  气相色谱-质谱法  腐乳  固相萃取

英文关键词:ethyl carbamate  gas chromatography-mass spectrometry  fermented bean curd  solid phase extraction

中文摘要:

      目的 建立一种固相萃取-气相色谱-质谱法(solid phase extraction-gas chromatography-mass spectrometry, SPE-GC-MS)检测腐乳中氨基甲酸乙酯的方法。方法 利用D5-氨基甲酸乙酯同位素做内标物, 样品用20%乙醇水溶液提取后, 利用碱性硅藻土固相萃取柱净化，洗脱液经浓缩后用气相色谱-质谱法测定样品中氨基甲酸乙酯。结果 该方法的加标回收率在88.8%~104.1%之间, 相对标准偏差( relative standard deviation, RSD)小于10%, 定量限为2.0 μg/kg(S/N=10)。结论 该方法提取效果好, 可以有效去除干扰物质, 检测灵敏度、准确度均满足检测工作要求。

英文摘要:

      Objective To establish a method for determination of ethyl carbamate in fermented bean curd by solid phase extraction-gas chromatography-mass spectrometry (SPE-GC-MS). Methods D5-ethyl carbamate was used as an internal standard substance. Samples were extracted with 20% ethanol water solution. The eluent was purified by solid phase extraction column of alkaline diatomite, and then was determined by gas chromatography-mass spectrometry after concentration. Results The recoveries of this method were 88.8%~ 104.1% and the relative standard deviations (RSDs) were below 10%. The limit of quantitation was 2.0 μg/kg (S/N=10). Conclusion The established method has good extraction effect and can effectively remove the interfering material. The sensitivity and accuracy of the detection can meet the requirements of the detection work.