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

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2.0μg/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。

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.