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2.0μg/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.
出处
《食品安全质量检测学报》
CAS
2018年第3期609-613,共5页
Journal of Food Safety and Quality
基金
郑州市科技创新团队计划项目(121pcxtd519)~~
关键词
氨基甲酸乙酯
气相色谱-质谱法
腐乳
固相萃取
ethyl carbamate
gas chromatography-mass spectrometry
fermented bean curd
solid phaseextraction